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二氧化钛(钛白粉)
二氧化钛(钛白粉). v1 _, V+ i1 j9 l
& w& R$ V& Q! e3 P7 NJECFA关于二氧化钛(钛白粉)的结论
Q$ }6 B3 |5 b! g7 h0 v( c9 R2 ~9 m" m9 W
摘要: 2006年JECFA关于二氧化钛的结论
: {5 D ?& i; i V5 f) I# cADI值:不作限制。
# G6 v$ i4 M( @( u功能:着色剂) J. ]' S* J1 e( H" {- p* k
* N r6 t0 [$ B1 w! y6 eTITANIUM DIOXIDE
3 m" D5 t5 w t( O% q3 wPrepared at the 67th JECFA (2006) and published in FAO JECFA
# t! {0 p( @1 y8 Q6 J9 hMonographs 3 (2006), superseding specifications prepared at the 63rd6 f( E& r8 b) Y/ p9 [% n
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the. B/ E" h6 Q: r1 [" C; m4 ]4 _% I: b
Combined Compendium of Food Additive Specifications, FAO JECFA
H+ d- r! `% _, G3 M* O# N7 xMonographs 1 (2005). An ADI “not limited” was established at the 13th4 G- e7 a2 [) e! q: c7 l" d+ Y0 K: m
JECFA (1969).1 B+ \6 \8 {# L7 O, m, X
SYNONYMS- T# Q9 \3 A# C6 o& c) K: C9 D+ L% f
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171, K+ k) e+ I2 s$ X
DEFINITION
- t2 @0 Q* D: A: [! _0 xTitanium dioxide is produced by either the sulfate or the chloride
4 N V6 n! V5 @1 w, fprocess. Processing conditions determine the form (anatase or rutile
0 W( c) l P0 P, |( u) Z3 c9 ?; s+ Astructure) of the final product.9 K- ?/ f$ S% H+ J- l# ?
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)) n2 f* j. b9 ], a$ I. w
or ilmenite and titanium slag. After a series of purification steps, the
# h; T( X/ D$ n, {3 visolated titanium dioxide is finally washed with water, calcined, and
8 t8 I7 S! W7 j! N! ?" d+ L2 O$ G5 s, omicronized.. [; }$ Z1 t- O/ t
In the chloride process, chlorine gas is reacted with a titaniumcontaining g1 t8 N, x J
mineral under reducing conditions to form anhydrous/ ^, z, Z+ x0 ^
titanium tetrachloride, which is subsequently purified and converted to
. |$ g* {+ y8 T# N- I8 I- ntitanium dioxide either by direct thermal oxidation or by reaction with
' }% D ]# |. d& n, y4 ]/ ?2 ~steam in the vapour phase. Alternatively, concentrated hydrochloric
$ n4 ]! ]5 g( Z/ t. X' ^9 N7 zacid can be reacted with the titanium-containing mineral to form a( `9 E, ?% A4 B) q. V F
solution of titanium tetrachloride, which is then further purified and4 R4 ~6 L1 U8 _" m* K- Y
converted to titanium dioxide by hydrolysis. The titanium dioxide is0 J Z& G$ Z! B! K% m
filtered, washed, and calcined.
( [& N) E/ ]* `" H0 E3 C' v1 n GCommercial titanium dioxide may be coated with small amounts of3 U% q# M3 \3 y: x; C/ ?8 J
alumina and/or silica to improve the technological properties of the' D: p0 y8 E1 T$ N7 D
product./ S% H$ I9 G) w. q
C.A.S. number 13463-67-7 i/ t$ c% H' g! R) g0 e8 b
Chemical formula TiO2$ H3 |+ [4 _" y4 c; `3 W0 Y: M$ d
Formula weight2 I' I4 V' F& r( j
79.88
# A/ L# U0 P7 O% b( N. |; [Assay
/ z4 a) U- ]" j- I- aNot less than 99.0% on the dried basis (on an aluminium oxide and
" B* Y) q8 a# R, {% _. W! @silicon dioxide-free basis)% w. ~% n2 i* v4 i& ^- ~
DESCRIPTION6 a+ e- ^8 ]9 }: I+ d
White to slightly coloured powder
$ ?% B" B) c W- ~* L/ KFUNCTIONAL USES1 F2 n8 [$ x1 _: G4 w' f0 t
Colour
" M. S. Y( m- }1 F% iCHARACTERISTICS* v7 Z- R# o% R/ N
IDENTIFICATION+ i3 j4 m. F1 e0 c4 O
Solubility (Vol. 4)
A- R+ W8 ^+ y2 n; \Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
/ ^2 L2 l/ d# G4 a) V. b6 w- Xsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
: s9 s' N7 _$ [1 l0 ^/ }sulfuric acid.
+ Y8 i6 l& N' H! T. \Colour reaction
- ]% l- |1 Z8 F! N( d% r1 eAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
$ B: {& j# h* L( ^0 o6 Qsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with% V$ M( ]1 w8 s$ N. b
water and filter. To 5 ml of this clear filtrate, add a few drops of
: U" I+ a% t0 y, Rhydrogen peroxide; an orange-red colour appears immediately.
9 c+ h7 W+ M1 b3 d7 {PURITY, a6 B6 B% H- e" k( H6 B& `
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
4 `9 l1 s( H/ Q' iLoss on ignition (Vol. 4). B- @8 u; c3 s" C# `* h
Not more than 1.0% (800o) on the dried basis
; c2 E+ a: q( o& W" Z$ d5 M* PAluminium oxide and/or
' T" _2 E# c4 g }' X; v; P. esilicon dioxide
}: R8 Z. x! }0 P) C# iNot more than 2%, either singly or combined5 z% `, A) I- r; U6 Q
See descriptions under TESTS6 k/ E: O0 s3 c5 P0 P5 I
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
/ d L* R% o9 _6 walumina or silica.2 _- r$ N1 x- G; Q# ?+ \* A& k
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and8 [" _5 S* t8 |$ M
place on a steam bath for 30 min with occasional stirring. Filter
. @; `/ M# W& y9 {/ M+ K6 y6 ythrough a Gooch crucible fitted with a glass fibre filter paper. Wash% k8 i, r2 \4 s/ |4 _8 r
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
9 d! u$ |0 A' Bcombined filtrate and washings to dryness, and ignite at a dull red# \- ~$ h/ Z# p% f: S. G$ j
heat to constant weight.) F6 \$ |: D$ H* d8 d8 |& E
Water-soluble matter
" ]! ]$ c& d. o9 }8 C: w2 Y(Vol. 4)9 v+ o* H1 D, b! F% q
Not more than 0.5%$ z Q$ K# b$ N0 p9 t# K
Proceed as directed under acid-soluble substances (above), using
$ A7 X4 r: V3 @water in place of 0.5 N hydrochloric acid.+ N; X6 a# ?* u% c4 X
Impurities soluble in 0.5 N
. ?1 R: O. O0 T3 }) _4 l* B. Y) s+ {7 bhydrochloric acid
+ s3 J/ @, h, LAntimony Not more than 2 mg/kg
: H' N k$ |. v# z- O; z# d4 U) nSee description under TESTS. P, a; y+ ^$ }% Z% S
Arsenic Not more than 1 mg/kg
4 ? z7 i) |1 b1 F, d' tSee description under TESTS
& Z$ F: N! w) j3 |. i3 e, vCadmium Not more than 1 mg/kg( `, u+ t* N8 \5 G! [
See description under TESTS
" V0 y$ c3 p, J I' R% ^; sLead
4 C" C3 Z* K; k: a$ N0 SNot more than 10 mg/kg9 y7 y( g0 L1 H) J4 u/ x1 u) _
See description under TESTS
5 v7 h9 E2 y3 JMercury (Vol. 4) Not more than 1 mg/kg9 v! Q: o$ a8 F! Y. @3 H) x$ @8 x
Determine using the cold vapour atomic absorption technique. Select a8 `, l8 D: p5 p8 M; w7 w( a& d8 G9 s
sample size appropriate to the specified level+ {+ r0 P# ^+ U+ @
TESTS2 S5 X5 {# {1 w, J6 x
PURITY TESTS
: z! o, |; r: u1 `% S6 AImpurities soluble in 0.5 N8 i7 X' o9 q# ?0 o- {
hydrochloric acid3 N" U/ H4 o- f0 t! B: E
Antimony, arsenic,' k! ^1 Z" p, |3 @" k. h- L) M
cadmium and lead
- @) ]9 e$ h" l a5 @ X% l(Vol.4)
/ w; t7 b7 J: A+ y6 R8 \9 ^# B2 T: yTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N- g1 Z7 Z; \& \
hydrochloric acid, cover with a watch glass, and heat to boiling on a
1 @4 W3 q* K# b) b$ rhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
0 M* ^1 H: b1 ^4 W3 F+ E+ p5 acentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
; {9 o. M. A( ?- v3 ?+ Kmaterial settles. Decant the supernatant extract through a Whatman
, I, r" Z% D8 ?8 |0 I# gNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml: j2 Y3 ?; l* F4 _" g$ o k4 L% {
volumetric flask and retaining as much as possible of the undissolved
. g Q0 P$ U6 \/ g# j; Mmaterial in the centrifuge bottle. Add 10 ml of hot water to the original9 I! C8 E7 G: w
beaker, washing off the watch glass with the water, and pour the
, j9 t7 v: z! _contents into the centrifuge bottle. Form a slurry, using a glass stirring
; N9 f. ?5 k1 ^rod, and centrifuge. Decant through the same filter paper, and collect9 M- B9 e, C+ r7 y, A" B0 \' N1 Y; W
the washings in the volumetric flask containing the initial extract.! r% f6 w* Y1 v- ?! c
Repeat the entire washing process two more times. Finally, wash the
; s8 c, g6 O& d3 Y& qfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask8 F/ W2 M3 q0 T6 s6 C4 P8 T$ n
to room temperature, dilute to volume with water, and mix./ b5 i9 n; E& d, D, U8 J7 `
Determine antimony, cadmium, and lead using an AAS/ICP-AES; Z# X# r" j" J7 M0 ~ S( t
technique appropriate to the specified level. Determine arsenic using the4 D0 w9 F4 `$ l3 j
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using, v% h0 A* Q( M) j5 [5 Z
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than# y8 P- m4 c; ~ s" _) c; F
1 g. The selection of sample size and method of sample preparation
* ^& M$ ~$ y* D: e( i+ }may be based on the principles of the methods described in Volume 4.8 R$ a1 V0 W- X% z3 H
Aluminium oxide Reagents and sample solutions& X0 N' ^. m& s* w N
0.01 N Zinc Sulfate: _2 y) I, L4 B
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to- A8 ~% c* { O5 B; A
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg! T# x( }0 p7 H7 Y
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
7 P7 L( \+ @% a; a" e" }& }' r" Rconcentrated hydrochloric acid, heating gently to effect solution, then9 q& q. x8 Q& r/ g. {! I# k
transfer the solution into a 1000-ml volumetric flask, dilute to volume
! O# K# e* Y& k$ ~with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
f3 m# g) K y" ]& }$ `" }ml Erlenmeyer flask containing 90 ml of water and 3 ml of
* V+ l( c+ G$ D o; N! Bconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
4 k6 g6 G* M" A# _) H; E( ~$ a/ @; _1 h25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,* }3 `5 g$ V% ?- x
dropwise, ammonia solution (1 in 5) until the colour is just completely
3 ]; N' ^$ ^2 E: [changed from red to orange-yellow. Then, add:2 n" r7 M0 F/ Y3 N
(a): 10 ml of ammonium acetate buffer solution (77 g of1 Z i% c% A* O" C! ?; P8 p; a. r
ammonium acetate plus 10 ml of glacial acetic acid, dilute to5 A1 B- R8 Q; b
1000 ml with water) and
- z, H! h7 H' v$ m$ a$ f8 L; f(b): 10 ml of diammonium hydrogen phosphate solution (150 g# d2 r1 l) E+ [# Y) a; d/ E
of diammonium hydrogen phosphate in 700 ml of water,6 U$ g7 E" }+ V6 O* g
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
3 U3 S$ C& N9 X* Q4 T6 Lthen dilute to 1000 ml with water).
5 A# R [ Y4 NBoil the solution for 5 min, cool it quickly to room temperature in a, ?! ~+ q+ r- n9 p$ B
stream of running water, add 3 drops of xylenol orange TS, and mix.
6 |" s& D7 u" j9 y$ F' E& N6 KUsing the zinc sulfate solution as titrant, titrate the solution to the first
+ Q& N2 z; c4 [ {yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
4 ~1 f* m& ^2 b& V1 m# WThis titration should be performed quickly near the end-point by$ n- Q! K- a0 e0 M) ^
adding rapidly 0.2 ml increments of the titrant until the first colour
3 `, E6 s! w1 U8 h! d1 X& {change occurs; although the colour will fade in 5-10 sec, it is the true' j, _8 S. C4 g+ y8 U: ^
end-point. Failure to observe the first colour change will result in an
& n2 }% y0 s8 ]9 N( L4 c& Z( e" Tincorrect titration. The fading end-point does not occur at the second
+ R- [) ?' t. Cend-point.)2 w. f+ R6 ]: o/ k: o# ]3 p8 X
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
! }7 j$ z' s* _% S- a; zstream of running water. Titrate this solution, using the zinc sulfate
5 m' n' g' ^5 g9 K* @8 W6 zsolution as titrant, to the same fugitive yellow-brown or pink end-point" d: K! J* r W1 w
as described above.
m% s4 S% O8 u, r* nCalculate the titre T of zinc sulfate solution by the formula:
! n r& p% |; H3 J% v6 S5 K! ST = 18.896 W / V" J! E; R3 B8 Q3 _! |" A
where
& b0 I Y0 C- j$ y; Z# A, x; F9 MT is the mass (mg) of Al2O3 per ml of zinc sulfate solution$ E1 o Q0 F! S2 O
W is the mass (g) of aluminium wire+ _2 i9 h/ q& T4 h' u2 |7 f/ @+ ?
V is the ml of the zinc sulfate solution consumed in the. |; f5 U7 _" W. T
second titration
8 @4 S+ R5 ~# W18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
* s* w! G; g) b7 ?9 @7 hR is the ratio of the formula weight of aluminium oxide to9 [7 ^7 E, @4 V1 S, h
that of elemental aluminium.
- j l9 n1 \/ L8 I3 MSample Solution A' ^5 B' C, V* A# d+ P1 v, q- @
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
0 T H2 d9 o+ B2 p3 Bglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
6 K: h) H; d/ D. D. F3 x" d# y, h(Note: Do not use more sodium bisulfate than specified, as an excess: T: H. [7 e( N
concentration of salt will interfere with the EDTA titration later on in the5 l1 ~) {) g- y. k- i0 e* {, n- S0 x
procedure.) Begin heating the flask at low heat on a hot plate, and9 y( O1 a5 w- n' g' f
then gradually raise the temperature until full heat is reached.: e" L; t! B4 V5 @7 E3 o7 J( R6 V9 I
(Caution: perform this procedure in a well ventilated area. ) When7 v; c, K: A2 @5 {+ G8 S7 x# A
spattering has stopped and light fumes of SO3 appear, heat in the full
" D; g1 W6 s1 [4 q, C+ H" S) lflame of a Meeker burner, with the flask tilted so that the fusion of the
0 L9 `. ~, p3 _. ]sample and sodium bisulfate is concentrated at one end of the flask.
; G- i: d! g$ p5 \, F% Y0 NSwirl constantly until the melt is clear (except for silica content), but8 j# k4 L6 ~. N( J! h
guard against prolonged heating to avoid precipitation of titanium/ P9 n3 G8 n/ o5 E$ G
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until. r" ]! \7 d# I
the mass has dissolved and a clear solution results. Cool, and dilute to
$ o6 e9 [/ e, e8 s# ~! q( D q, R \120 ml with water. Introduce a magnetic stir bar into the flask.$ ~! f6 |* w/ U% G( L) e2 Q, r
Sample Solution B
9 x( [$ |* c {Prepare 200 ml of an approximately 6.25 M solution of sodium
( v/ W& ?7 q' g$ D r% N6 {hydroxide. Add 65 ml of this solution to Sample Solution A, while& _, ?' T: M8 ]2 `# ]* m1 `
stirring with the magnetic stirrer; pour the remaining 135 ml of the
- Y8 ]0 A- w4 K4 e: Valkali solution into a 500-ml volumetric flask." _ R5 f/ U9 Z; i: K/ v
Slowly, with constant stirring, add the sample mixture to the alkali
! d8 I! T$ s" p) _# s2 R& ssolution in the 500-ml volumetric flask; dilute to volume with water,- @, `7 D: B/ c) }
and mix. (Note: If the procedure is delayed at this point for more than
6 G& J. a% M& u6 f* [. S2 hours, store the contents of the volumetric flask in a polyethylene: r+ V3 A. y- h8 \3 b9 ?1 G$ a
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),( J: @ J- P: P) k0 G
then filter the supernatant liquid through a very fine filter paper. Label! o& j# a+ b! y6 Y5 ]" g7 c! w
the filtrate Sample Solution B.
( g# Q' o" W+ E3 L% n$ ]+ w) H9 SSample Solution C
- ^" F- ]4 r0 DTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
: z' X- Y& ~% d4 C) c Y5 \# mflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
6 C& S5 W7 M2 b) B. ssolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
. f [7 e7 p; C8 EM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is9 E& r# V m1 D* K
known, calculate the optimum volume of EDTA solution to be added
7 c$ w0 Z( X k. {4 @2 Y+ ]by the formula: (4 x % Al2O3) + 5.]
& h& Z0 A5 Z+ c# ~" YAdd, dropwise, ammonia solution (1 in 5) until the colour is just# [0 J" {- C6 O. t- M: y
completely changed from red to orange-yellow. Then add10 ml each
5 }' G, G9 J( S+ c2 Fof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
8 @3 m( _3 ?, p" Sroom temperature in a stream of running water, add 3 drops of xylenol
5 ?! E, m/ ?6 r% `5 m' iorange TS, and mix. If the solution is purple, yellow-brown, or pink,, _9 r9 N8 l8 H8 W
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
- B3 a3 k. z+ `8 @pH, a pink colour indicates that not enough of the EDTA solution has
0 ?% A% c8 J! i# Tbeen added, in which case, discard the solution and repeat this
* p( Z9 U' X0 Y- }procedure with another 100 ml of Sample Solution B, using 50 ml,
1 Z. K- w& T w9 j- Z; qrather than 25 ml, of 0.02 M disodium EDTA.
' Z1 |6 j5 s9 H% SProcedure5 `# L' r% K$ V) g3 n% s
Using the standardized zinc sulfate solution as titrant, titrate Sample
! W2 V: P* ^- }# L- eSolution C to the first yellow-brown or pink end-point that persists for
1 g: u" Q8 f: m3 C5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first2 W- ~! w3 _4 B- j
titration should require more than 8 ml of titrant, but for more accurate, p$ L9 U+ b0 }3 |, d5 o
work a titration of 10-15 ml is desirable.
, Q8 z$ L' d, g" KAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
+ R$ c1 K! x; O' wmin, and cool in a stream of running water. Titrate this solution, using: s3 i' F5 k9 l4 e6 \
the standardized zinc sulfate solution as titrant, to the same fugitive5 V9 E8 E+ I6 U; o+ e5 k* s& X
yellow-brown or pink end-point as described above.5 o# f0 j* W( w8 M9 y& j W
Calculation:
1 j2 y- g" F' cCalculate the percentage of aluminium oxide (Al2O3) in the sample
% Z+ e; L1 C# V% y. Dtaken by the formula:
5 T) a# s; `, g* p9 m% Al2O3 = 100 × (0.005VT)/S2 Q9 v6 K; T+ ^1 Z
where
4 S+ N" ?: k/ @! e/ k1 ^' oV is the number of ml of 0.01 N zinc sulfate consumed in
8 s: N% r: |# | P& ithe second titration,
2 F' d# r3 s3 B# W1 _+ {T is the titre of the zinc sulfate solution,
) T( d" J- x7 U" R5 T' {S is the mass (g) of the sample taken, and
. C- v, C. }3 J+ F8 f0.005 = 500 ml / (1000mg/g × 100 ml).* U% ^% m1 t5 w' u% a
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica, G5 h, S# R# q. S6 u2 d
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).5 k, k% H# p8 |
Heat gently over a Meeker burner, while swirling the flask, until
J8 m% f2 }: x, G2 adecomposition and fusion are complete and the melt is clear, except
) }4 \" z7 L1 N2 A+ Gfor the silica content, and then cool. (Caution: Do not overheat the, y" o7 }9 s& E$ B6 a8 ^+ ` J
contents of the flask at the beginning, and heat cautiously during5 Z9 G, c) J5 M6 D3 c
fusion to avoid spattering.)1 Q9 q2 }. L9 o, q2 d, w& E
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat' k4 c+ h" C/ y5 ~" d6 X
carefully and slowly until the melt is dissolved. Cool, and carefully add
3 V! o5 t0 b2 X+ a. t- H$ x0 N150 ml of water by pouring very small portions down the sides of the
' k2 o$ W% [* i# F2 Y. |flask, with frequent swirling to avoid over-heating and spattering. Allow J! C2 J: }4 Y# {; A4 h! J M: Q7 k
the contents of the flask to cool, and filter through fine ashless filter4 p+ ]; V' q6 T I! k; ~& D
paper, using a 60 degree gravity funnel. Rinse out all the silica from
1 \9 g5 y; |( m" f; _ u4 y0 Tthe flask onto the filter paper with sulfuric acid solution (1 in 10).
; f" c+ |/ a; y+ }/ y f" VTransfer the filter paper and its contents into a platinum crucible, dry in
# I9 M, o4 _# ^6 Y, x3 o4 M: B% qan oven at 1200, and heat the partly covered crucible over a Bunsen& ?- u7 j% i9 u+ J! s+ M6 A
burner. To prevent flaming of the filter paper, first heat the cover from4 [; d$ _4 J- J1 F$ D
above, and then the crucible from below.
6 r, }! D; `& {) w9 ~0 dWhen the filter paper is consumed, transfer the crucible to a muffle4 w/ O) o8 L" _3 o8 h) @ w
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and0 q1 }! K% z: s9 M9 w! B' v
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated; S D5 v2 k2 \
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first: \! _( W: l# P `( T
on a low-heat hot plate (to remove the HF) and then over a Bunsen6 E8 P, l! [7 T6 o6 i0 a* H6 B# A
burner (to remove the H2SO4). Take precautions to avoid spattering,4 Z* \; g0 Z; t0 v* U
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
3 j' ^$ C+ v" u/ _' [1 W$ m9 o- vdesiccator, and weigh again. Record the difference between the two" C0 l0 Z% c I. ~
weights as the content of SiO2 in the sample.
' s7 g2 I- q( SMETHOD OF ASSAY& t" R& L, r7 u- J3 c; I7 }
Accurately weigh about 150 mg of the sample, previously dried at 105o
4 L) a, D2 g& }; Mfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
5 t, Y% C. D% d; @and shake until a homogeneous, milky suspension is obtained. Add 30# t7 d& k( F7 o) V* `. v- o
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
8 F F) _! d: G% xheat gently, then heat strongly until a clear solution is obtained. Cool,. J8 S/ O- p8 B; I! N
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric5 _: w2 {3 ]# q% m$ k: l$ Q
acid, and stir. Add 3 g of aluminium metal, and immediately insert a# H1 h$ |) [. g$ F g# n
rubber stopper fitted with a U-shaped glass tube while immersing the7 b* i! G, k6 C3 y! c) t! ^9 p
other end of the U-tube into a saturated solution of sodium
" X! f+ ~5 j( J& b( s1 P5 R, zbicarbonate contained in a 500-ml wide-mouth bottle, and generate
. u# _: p2 u4 H+ q5 Rhydrogen. Allow to stand for a few minutes after the aluminium metal
" D" }4 q2 B* A& R2 k- e ~has dissolved completely to produce a transparent purple solution.
4 G0 T" K0 g0 A) N' f S4 [8 o; qCool to below 50o in running water, and remove the rubber stopper y5 ^. K: _! A' [9 i! \
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
+ Z: k0 L1 I/ asolution as an indicator, and immediately titrate with 0.2 N ferric
9 B& K6 o# `6 \9 P) N0 \ammonium sulfate until a faint brown colour that persists for 30
, n/ C8 D7 C5 n" q. D. J3 Vseconds is obtained. Perform a blank determination and make any2 q: \6 V/ V$ y4 t+ n' V o8 N) I
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
: G/ {+ ` @3 C6 zequivalent to 7.990 mg of TiO2.# C" R2 i- e3 v* q5 ~3 E( Z; T X1 y4 t
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