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二氧化钛(钛白粉)
二氧化钛(钛白粉)' A3 _! r& m9 [! p0 \
/ A% H; `- g; J- lJECFA关于二氧化钛(钛白粉)的结论7 T5 u+ F5 q& z; ?/ B4 ^
- W1 H7 \- V8 V% h* c$ a' V摘要: 2006年JECFA关于二氧化钛的结论
3 J' {" o6 ]7 Q9 U- O& d3 l/ yADI值:不作限制。
+ c0 l+ S- ?5 X4 S; k功能:着色剂
% c+ L- _/ m" j* o+ d/ A! H# w' }2 S( |- t9 I
TITANIUM DIOXIDE
' X W* s- G* j! |Prepared at the 67th JECFA (2006) and published in FAO JECFA
2 O0 N. y3 ]+ Q, S7 SMonographs 3 (2006), superseding specifications prepared at the 63rd9 |! m3 [9 Z4 S; e- A/ b2 \1 n& i
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
( q6 q8 S- V n5 d: ACombined Compendium of Food Additive Specifications, FAO JECFA
/ C" D+ ?: C, m( nMonographs 1 (2005). An ADI “not limited” was established at the 13th
/ d7 E2 N- u! z0 ?JECFA (1969).0 ~) F$ N' p6 @! S7 p y U' L
SYNONYMS
8 Y( p7 M$ ~( T) W& BTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171; l1 e% x% u6 U# n9 c* m, C
DEFINITION4 K* n9 N5 Q2 g9 a/ R6 _
Titanium dioxide is produced by either the sulfate or the chloride
/ W# g- X5 `- D) C* ^0 l& lprocess. Processing conditions determine the form (anatase or rutile) Y+ c& ]- b: F' i2 i! U) ?& \
structure) of the final product.: l7 Q. r! o) O+ @
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
$ A. c8 t* e' a* J7 z9 Lor ilmenite and titanium slag. After a series of purification steps, the6 ?) P" n7 J; D8 k9 Y
isolated titanium dioxide is finally washed with water, calcined, and1 A, s# W- {8 }3 M4 e6 r3 s
micronized.
" j. c3 J) Z6 [8 CIn the chloride process, chlorine gas is reacted with a titaniumcontaining* `- J8 V: P! a' f
mineral under reducing conditions to form anhydrous0 W! O/ x/ U, H" O
titanium tetrachloride, which is subsequently purified and converted to5 C: ? z$ x+ w1 _/ K
titanium dioxide either by direct thermal oxidation or by reaction with# T" s5 ^# x. q& P# }- l
steam in the vapour phase. Alternatively, concentrated hydrochloric
& {6 d- W* n3 d; N4 jacid can be reacted with the titanium-containing mineral to form a& T! q. H1 @' E& E1 w3 v
solution of titanium tetrachloride, which is then further purified and2 o2 Z) [- L q2 R. m
converted to titanium dioxide by hydrolysis. The titanium dioxide is
C3 N" X; \( ?" O& ^2 R; gfiltered, washed, and calcined.6 n9 d8 |# E+ M! z# k. O8 u
Commercial titanium dioxide may be coated with small amounts of0 A5 X4 {) q" {
alumina and/or silica to improve the technological properties of the
7 N# Z) y2 J0 A- q, c1 O$ `product.; r2 U# l8 @ h' Z- Z7 A8 V
C.A.S. number 13463-67-7
) e2 c) e( h! ?8 u3 T6 uChemical formula TiO2
* g# @6 J! F: @* X, RFormula weight
+ D' C4 ]- C; N/ `& H: J79.88
) N- e x+ @( ?" i4 u( jAssay+ U7 U, s* B$ X& k; t4 P$ y8 e' ?% a0 c" Y
Not less than 99.0% on the dried basis (on an aluminium oxide and
, {- O; k- h* g( j! ksilicon dioxide-free basis)
5 R4 F4 Y7 I5 \( v% H! CDESCRIPTION
, K% e: B: @ N: b) n# p. _0 O$ GWhite to slightly coloured powder- f2 w5 O) A+ U
FUNCTIONAL USES3 a6 ]; ?1 W6 G' H- p0 ^( i) V' K: O3 o/ q
Colour
# \7 J J, W% e5 B$ T! }: L; _. nCHARACTERISTICS
; Y9 |4 `# h& j _. c WIDENTIFICATION! K2 N: |8 \* r. {: H
Solubility (Vol. 4)
/ c6 `0 W9 N. {6 U4 gInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic/ D8 V! e' G, n8 D" M8 _
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
& _( o' }* h/ V+ z- Fsulfuric acid.
+ G9 c0 ~" O5 ]* {8 |) U) {& ?Colour reaction
$ }$ H: U6 p9 {9 G$ c# MAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
! ?( W* N2 ?4 u+ E! z7 v8 Osulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
" [: v2 r8 B( b" s. t7 D: Bwater and filter. To 5 ml of this clear filtrate, add a few drops of
* G4 n2 o: P2 m+ X! W w( Z; Jhydrogen peroxide; an orange-red colour appears immediately.; s* V& j2 P5 m+ Z4 F
PURITY
6 w t% W9 W' ? RLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
4 O n, T! U- b0 rLoss on ignition (Vol. 4)
) |; Z; p, `! p# PNot more than 1.0% (800o) on the dried basis, W* {! R/ a8 }( l& P& `/ O
Aluminium oxide and/or
^, b/ ^, k. Y9 esilicon dioxide
% Z( c) c+ R1 e% e* @6 I$ I3 o! FNot more than 2%, either singly or combined
/ F4 A" r& r0 \; b' zSee descriptions under TESTS! o; ?- |. n9 |) {6 Y
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
0 n1 A1 L5 O9 ^ halumina or silica.
6 f" A" v! ~2 ^6 xSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and& A2 K* E- z- Z0 t
place on a steam bath for 30 min with occasional stirring. Filter
; W* P. {" S& s' _through a Gooch crucible fitted with a glass fibre filter paper. Wash
; H( @0 u+ R& x1 Zwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the: {* R5 D' O& T$ g q m
combined filtrate and washings to dryness, and ignite at a dull red% F9 N, e' V \, u/ b7 v
heat to constant weight.
9 M+ W0 x2 K; i. VWater-soluble matter! _/ F9 r, T5 F, O9 p
(Vol. 4)" h8 u) V2 z9 m8 G/ u
Not more than 0.5%
/ x$ d' v- n" e* X5 N$ r+ GProceed as directed under acid-soluble substances (above), using" D$ T% x _. h3 D
water in place of 0.5 N hydrochloric acid.' }# @/ s; }6 x# C- d- t- p
Impurities soluble in 0.5 N
3 l, F' X+ N: u8 q) q6 ^% Qhydrochloric acid; N7 D4 n( R- Q( u
Antimony Not more than 2 mg/kg
; v2 f4 u5 j7 m2 {1 N0 R" bSee description under TESTS- x( u6 e9 d% r$ @( B x; |
Arsenic Not more than 1 mg/kg/ T% i$ _4 x5 ?2 b2 u
See description under TESTS
$ g" L0 L$ k1 I3 O/ X4 zCadmium Not more than 1 mg/kg
5 c! M- X& }, E4 d, M* aSee description under TESTS
% D2 H1 k+ H3 O: BLead5 i! p: b; a2 Q v9 p2 Z
Not more than 10 mg/kg
+ e% A, T M; t% I) v; H" ?5 }See description under TESTS
6 I! M6 y: R5 q+ jMercury (Vol. 4) Not more than 1 mg/kg( m9 z2 `1 q2 r2 x$ I$ ~
Determine using the cold vapour atomic absorption technique. Select a
/ V" ?. K+ X" ?1 X: ]( F) ]sample size appropriate to the specified level( A& g O8 \( r, V' S
TESTS
7 r9 z1 @/ M8 @/ Q$ U, W( KPURITY TESTS
* [( {7 |; R6 P& Q: ?8 b0 AImpurities soluble in 0.5 N8 {7 `; [4 p' P% u) I( L8 L
hydrochloric acid* `' N) S8 e+ n% L/ ^
Antimony, arsenic,: D2 I0 {6 p2 x: h+ G3 ^
cadmium and lead
4 X9 D% D4 T! W j9 M(Vol.4)
4 Z/ z4 e' O; o4 `( [: x0 {0 tTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N+ @( ^$ Y, B* O% Z; m* L
hydrochloric acid, cover with a watch glass, and heat to boiling on a( o: X4 P% r. `: Y! ^4 a: t
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
3 B/ j- p9 Z1 ]0 E4 @centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
; [# l' `" D% }; Y+ U4 imaterial settles. Decant the supernatant extract through a Whatman& y# r2 u2 L" A( k1 F6 J$ I1 U4 Z: R! r
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml: w4 c& v3 b2 l( o/ M% l& h6 @
volumetric flask and retaining as much as possible of the undissolved4 |6 Y" A' X7 o! q. D0 \5 ?
material in the centrifuge bottle. Add 10 ml of hot water to the original* `' A# ~- R8 a& J4 Q: ]* a
beaker, washing off the watch glass with the water, and pour the9 `6 j; a- D1 c" V
contents into the centrifuge bottle. Form a slurry, using a glass stirring9 _( G" W S+ P5 |/ x2 s" ~% B! f
rod, and centrifuge. Decant through the same filter paper, and collect! {/ q( b. [& _9 {1 [: s' {, [& l
the washings in the volumetric flask containing the initial extract.
- G, `9 X% v" @2 \$ k- g$ S6 oRepeat the entire washing process two more times. Finally, wash the
8 _. U" E; x# u+ n% i. e5 K$ _filter paper with 10 to 15 ml of hot water. Cool the contents of the flask5 o' h; @ f& I8 V! z7 Z. g
to room temperature, dilute to volume with water, and mix.: A, D; c; t9 n- V! g2 s
Determine antimony, cadmium, and lead using an AAS/ICP-AES
7 S' k. u$ ]( F$ }$ ctechnique appropriate to the specified level. Determine arsenic using the. x5 g) K( `0 o" U% @$ Z/ r, L- M
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using$ a% T+ C. C! t9 ]
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than! h; F6 F1 \" u \4 h
1 g. The selection of sample size and method of sample preparation- K# i3 ~6 K/ V# ]$ Y
may be based on the principles of the methods described in Volume 4.9 G5 F3 G4 k+ X$ g- F
Aluminium oxide Reagents and sample solutions
; |9 @5 L9 O: N1 q, X0.01 N Zinc Sulfate" x/ k `" t& h. L, Q5 ]
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
' P/ W/ W4 j, a5 ^. B% @) @# p6 Qmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg( d1 U5 N* \' K) W: s* c
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
5 `* A) o3 i: z+ n& g9 r, jconcentrated hydrochloric acid, heating gently to effect solution, then
7 Y. \# u2 M) S+ mtransfer the solution into a 1000-ml volumetric flask, dilute to volume1 U) u p: Y5 J9 I! h
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5005 C6 x0 M; C2 j* ?4 A* W- b
ml Erlenmeyer flask containing 90 ml of water and 3 ml of ^1 w3 p9 ~) m
concentrated hydrochloric acid, add 1 drop of methyl orange TS and* p6 t- Z' B0 D* x' L( B
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,# g! Y4 `/ e& b. O: U; f$ ` D
dropwise, ammonia solution (1 in 5) until the colour is just completely
9 {) X0 J) |& T2 X' T2 a5 wchanged from red to orange-yellow. Then, add:
4 Y3 b6 J5 n- S( g4 ]" x3 J(a): 10 ml of ammonium acetate buffer solution (77 g of6 b: ?+ V3 n. k4 y2 W0 D& Y8 M
ammonium acetate plus 10 ml of glacial acetic acid, dilute to# g! e( x2 O, P" @
1000 ml with water) and' F, \( P7 M F# }# u+ ?8 O
(b): 10 ml of diammonium hydrogen phosphate solution (150 g9 d9 w3 M6 u$ s0 s( O
of diammonium hydrogen phosphate in 700 ml of water,
1 e6 v# m! b* c+ C5 kadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,# t0 p: Q6 m/ I) Y8 m
then dilute to 1000 ml with water).
9 U9 w) l( j4 JBoil the solution for 5 min, cool it quickly to room temperature in a
" T2 z( ^) k) Z2 cstream of running water, add 3 drops of xylenol orange TS, and mix.
1 i& j! u3 Z3 f, I4 UUsing the zinc sulfate solution as titrant, titrate the solution to the first
4 I: y v3 @4 syellow-brown or pink end-point colour that persists for 5-10 sec. (Note:" O; Z* e+ n( Q7 E2 ^2 i7 J' F, F
This titration should be performed quickly near the end-point by6 R6 _$ O: O \8 X' `
adding rapidly 0.2 ml increments of the titrant until the first colour; C6 b0 Y! l) C( a
change occurs; although the colour will fade in 5-10 sec, it is the true( e1 z" y. D& B d+ T
end-point. Failure to observe the first colour change will result in an
~0 q6 p% o, D* F( L: xincorrect titration. The fading end-point does not occur at the second# p. y( u: W4 B/ O( w0 W
end-point.)- T/ _- H4 l2 g2 t& i
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
# i! W9 S7 h# `6 vstream of running water. Titrate this solution, using the zinc sulfate* Z( O; `3 H# f& f- i! z
solution as titrant, to the same fugitive yellow-brown or pink end-point
& X9 r& |3 ?" K+ e$ V7 s- mas described above.+ c( |6 R6 i3 N% i2 O. Y
Calculate the titre T of zinc sulfate solution by the formula:- n& m$ S6 S% A2 L7 @5 F
T = 18.896 W / V) V, T4 t$ B" A% {0 {
where
' r1 K G' T3 k3 k- yT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
; ^$ G, b$ d% Y7 ]/ uW is the mass (g) of aluminium wire4 s' F. R# H! w, ]. E' \% Z
V is the ml of the zinc sulfate solution consumed in the7 d2 n" d7 N7 v1 S
second titration
. \ N$ H$ L) j ~18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
9 ^7 L/ f% v7 i+ ~! u) GR is the ratio of the formula weight of aluminium oxide to
) [' Y- e7 u0 J; p2 B5 lthat of elemental aluminium.* o* P. ?. o. y& m2 n( h
Sample Solution A
) X- z( U2 O) r# L- |8 kAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
' v- T: n; [) x% K# gglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
3 |. O- c0 b* p6 v; _7 V0 h- f(Note: Do not use more sodium bisulfate than specified, as an excess+ P9 O7 u8 T$ M% F& k! o
concentration of salt will interfere with the EDTA titration later on in the
- l5 y' c5 Q A# n/ a. Eprocedure.) Begin heating the flask at low heat on a hot plate, and: d! s! g; C; L
then gradually raise the temperature until full heat is reached.$ f; k/ W9 v6 `+ \* W4 x% d
(Caution: perform this procedure in a well ventilated area. ) When
& P1 _1 Q, N0 y4 I) {. Hspattering has stopped and light fumes of SO3 appear, heat in the full
2 J; }% [+ m, jflame of a Meeker burner, with the flask tilted so that the fusion of the
. K0 V* e- p4 D( h1 b% ]0 \, h: dsample and sodium bisulfate is concentrated at one end of the flask.- [5 P8 m0 ]8 w0 k/ i2 V# D
Swirl constantly until the melt is clear (except for silica content), but
- |1 x9 c% E4 O! R+ y1 Jguard against prolonged heating to avoid precipitation of titanium
, z( v+ L6 C/ V, ~4 m Hdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
4 V# c9 p# B' i0 hthe mass has dissolved and a clear solution results. Cool, and dilute to; j1 @9 i& O$ \
120 ml with water. Introduce a magnetic stir bar into the flask.8 N+ C. a& @2 u+ l3 l
Sample Solution B
( |1 p' T5 p, ^( L: j. w7 y6 _. sPrepare 200 ml of an approximately 6.25 M solution of sodium
) ~ _ m7 R; J4 X+ O1 y: t- Khydroxide. Add 65 ml of this solution to Sample Solution A, while* w7 N0 T x6 n/ n5 X5 \' e% m4 H1 j
stirring with the magnetic stirrer; pour the remaining 135 ml of the
& ? s; Y% X" Y9 }6 O; jalkali solution into a 500-ml volumetric flask.
6 Q$ i5 D* E" p2 G5 @8 ]# j, ESlowly, with constant stirring, add the sample mixture to the alkali
2 y' l, h" e+ s- p" [2 psolution in the 500-ml volumetric flask; dilute to volume with water,
( `* A% ^# i e+ Vand mix. (Note: If the procedure is delayed at this point for more than' {9 X; J) p+ w: V( V
2 hours, store the contents of the volumetric flask in a polyethylene
; [; k) @; p* g6 bbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
* T" n+ `# s1 q! Dthen filter the supernatant liquid through a very fine filter paper. Label
. g6 W& x1 s n9 G- ]9 b4 I- o+ }the filtrate Sample Solution B.
% K9 A8 L) E* L7 X2 [ HSample Solution C
/ v1 K0 Q8 ~- ?5 `: F hTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer* a2 u; f2 H' o( c
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
2 a) T8 U0 H$ f: vsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
$ u9 ?. k% O5 J8 F; d: pM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
, I9 B3 X% L0 [; j0 p1 Mknown, calculate the optimum volume of EDTA solution to be added" [0 e4 k- \% [4 O$ ~
by the formula: (4 x % Al2O3) + 5.]8 m9 u( k% q" k1 z: ]: v
Add, dropwise, ammonia solution (1 in 5) until the colour is just
' v: v: ?" ?1 ^9 Icompletely changed from red to orange-yellow. Then add10 ml each
1 Q* I# q, x8 R& w3 @4 K# uof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
1 m% a$ h7 x/ O8 V1 Yroom temperature in a stream of running water, add 3 drops of xylenol
! y/ ~! \5 K! zorange TS, and mix. If the solution is purple, yellow-brown, or pink,
: U1 }4 g8 r7 d& abring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired% t3 w5 C: x! c" V6 I8 ~. u& I
pH, a pink colour indicates that not enough of the EDTA solution has
( O0 I/ x/ c: A" A! G. S' Abeen added, in which case, discard the solution and repeat this! K+ D( i, l# t! h9 {2 p9 }
procedure with another 100 ml of Sample Solution B, using 50 ml,
; i, l5 g* ^8 A# v3 s9 ^+ Qrather than 25 ml, of 0.02 M disodium EDTA.
" q1 y: Q. b- e& S0 z. uProcedure
2 Y3 r' V0 G5 [5 {Using the standardized zinc sulfate solution as titrant, titrate Sample
/ m: P% \; x& ]+ ], V, K+ I% ySolution C to the first yellow-brown or pink end-point that persists for1 ~9 } M4 e5 O1 G e' ?
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
( l( L* G6 g4 R0 r* i. ttitration should require more than 8 ml of titrant, but for more accurate; L3 X H3 u# T x# M
work a titration of 10-15 ml is desirable.2 g% F1 q. a0 n
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
% z- p, ^4 j9 O) p) H; _min, and cool in a stream of running water. Titrate this solution, using
) J7 A6 ]2 { V, n: A4 wthe standardized zinc sulfate solution as titrant, to the same fugitive8 `( {+ ^( z! }$ u& s6 t
yellow-brown or pink end-point as described above.
2 `' T& \* S* L B) y3 T) w$ u/ P$ ?Calculation:6 U+ a. ]8 H6 P: L" M' U1 ~
Calculate the percentage of aluminium oxide (Al2O3) in the sample ^) N# ]" R3 Q% K0 G" N
taken by the formula:0 x" f5 s% x' t8 ~
% Al2O3 = 100 × (0.005VT)/S
' Q- F$ b/ ^) ?3 E# D- T$ Y- lwhere1 W, O, _ G% {' @- @$ @
V is the number of ml of 0.01 N zinc sulfate consumed in3 A( S2 K$ M9 R1 b8 }
the second titration,
6 g* P: @' `$ e4 b9 vT is the titre of the zinc sulfate solution,
4 p; a8 x, _ q* pS is the mass (g) of the sample taken, and
" _7 E/ ~6 {8 ?+ O9 J* r$ r; A0.005 = 500 ml / (1000mg/g × 100 ml).+ X6 V& y8 @) K, Z
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica; q" }# D. g( w' l1 H! k a
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).6 Y! w5 e5 }) @" Q/ _3 Y
Heat gently over a Meeker burner, while swirling the flask, until
- v# I+ G8 j: v) rdecomposition and fusion are complete and the melt is clear, except
) ?4 S. w( s8 x/ y- @' ofor the silica content, and then cool. (Caution: Do not overheat the
+ s9 ?& s: s6 R# d8 V! T0 ^! ucontents of the flask at the beginning, and heat cautiously during2 T H. \7 t; X8 p3 M
fusion to avoid spattering.): l3 H. f& V5 Q* G0 U
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat' ^) A. U6 c$ u: ^) U4 h; a( W2 D
carefully and slowly until the melt is dissolved. Cool, and carefully add% i4 p( S- P E7 Y) G- B, p
150 ml of water by pouring very small portions down the sides of the
! H& v, {; U* cflask, with frequent swirling to avoid over-heating and spattering. Allow3 Z" J0 @7 X2 R
the contents of the flask to cool, and filter through fine ashless filter
' p) N# y+ j% xpaper, using a 60 degree gravity funnel. Rinse out all the silica from. T m/ K8 j# u
the flask onto the filter paper with sulfuric acid solution (1 in 10).8 I6 q6 H: B+ J* n: C; m7 \2 c
Transfer the filter paper and its contents into a platinum crucible, dry in. A, P7 j1 W/ Q3 w4 R% n
an oven at 1200, and heat the partly covered crucible over a Bunsen% I: ?6 \6 ~( d' ^" T1 Q: ~9 z
burner. To prevent flaming of the filter paper, first heat the cover from4 C' p9 J( ~8 Z3 r$ m) D
above, and then the crucible from below.; C& s1 Q" a7 q
When the filter paper is consumed, transfer the crucible to a muffle4 U( E* B7 C7 A* [8 Y8 b
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
9 i9 V$ ?3 w/ c7 a' |5 S7 l+ M5 oweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated$ U. H: \0 x6 |1 g$ h4 H
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first( B6 a/ `7 H& ^& ?5 f) D
on a low-heat hot plate (to remove the HF) and then over a Bunsen- }4 A0 I! l) O
burner (to remove the H2SO4). Take precautions to avoid spattering,
2 A( m2 K' w' }especially after removal of the HF. Ignite at 1000o for 10 min, cool in a, h" m# q: G2 L
desiccator, and weigh again. Record the difference between the two
/ n7 ]3 E* p# Xweights as the content of SiO2 in the sample.7 l( u1 s$ j% \( w5 Q
METHOD OF ASSAY
! o, i& }5 y* p0 NAccurately weigh about 150 mg of the sample, previously dried at 105o0 }, p9 X8 J8 K) N% R' d( A
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
7 O; m/ b4 X* Y$ B9 }, N+ H- cand shake until a homogeneous, milky suspension is obtained. Add 30" h3 |( l3 _4 t1 u
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
0 k5 l0 X# f) ^: Y3 Eheat gently, then heat strongly until a clear solution is obtained. Cool,
8 S0 `2 I; v$ F! Ethen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
6 u. L; P* D. ~1 T# A+ T, facid, and stir. Add 3 g of aluminium metal, and immediately insert a
. `2 s+ b( e5 N; arubber stopper fitted with a U-shaped glass tube while immersing the
2 s) b+ k0 D# e$ O3 s! ^/ Bother end of the U-tube into a saturated solution of sodium
3 a. h/ I q" w8 x1 [bicarbonate contained in a 500-ml wide-mouth bottle, and generate
_: ]7 U: P4 I5 L$ w% @! zhydrogen. Allow to stand for a few minutes after the aluminium metal' T% z+ o6 D c3 Q( q1 X+ f" V
has dissolved completely to produce a transparent purple solution.
% e4 P1 _8 D) a5 kCool to below 50o in running water, and remove the rubber stopper/ l" p/ v5 l* W q
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate7 x: t; r% i7 u$ x8 \- h
solution as an indicator, and immediately titrate with 0.2 N ferric
P$ Z/ x v7 P5 q& S2 U+ Z! tammonium sulfate until a faint brown colour that persists for 30. B- V& S) D2 @) ~1 [( V: R" s' D
seconds is obtained. Perform a blank determination and make any2 }1 U( p) I( o
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is s- _9 }0 {! I0 g* ~* p
equivalent to 7.990 mg of TiO2.
2 p* g/ }6 u+ b! b3 ]0 V1 u7 g, }7 a |
|