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二氧化钛(钛白粉)
二氧化钛(钛白粉)4 P( I: ]* ^4 f" p/ w3 Z/ \) [" I1 x
+ B8 [4 b. v8 d8 ^3 e' z5 d6 k% wJECFA关于二氧化钛(钛白粉)的结论
/ M, k, @/ b% \+ P
3 ~6 _ W, a; ^( D, d摘要: 2006年JECFA关于二氧化钛的结论3 d/ p* \" T: J1 ?
ADI值:不作限制。! Z& L a5 J" T+ {
功能:着色剂& a8 I' M* X: ?6 Y- I* h
1 j6 u3 ^( ~* U0 R1 {+ V$ I, V
TITANIUM DIOXIDE6 ~! Z# d% p& [* U
Prepared at the 67th JECFA (2006) and published in FAO JECFA$ U+ }2 o" V( m* }# h7 b* {$ I
Monographs 3 (2006), superseding specifications prepared at the 63rd
5 U4 M0 W3 }5 i/ z4 kJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
/ f1 P( Z4 `: K* jCombined Compendium of Food Additive Specifications, FAO JECFA3 C$ e; R/ i9 _, n- _
Monographs 1 (2005). An ADI “not limited” was established at the 13th
( u9 u" d8 ~; L8 V3 e( ]JECFA (1969).
( L7 m( J) X% USYNONYMS9 r7 d7 y1 F- S' h& \* I
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171( v; N2 f" P4 h2 R& P
DEFINITION+ U3 Y0 G, t+ t0 o F' A
Titanium dioxide is produced by either the sulfate or the chloride
6 C/ y9 _) @4 n7 K# z' I- W4 Kprocess. Processing conditions determine the form (anatase or rutile: F" y8 U0 i5 o+ h$ G: h
structure) of the final product. {4 q2 W6 M+ K' u% B: |: F( c
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
! F q2 ~8 A. m# h% b& Por ilmenite and titanium slag. After a series of purification steps, the
& j; t. r* }# g: xisolated titanium dioxide is finally washed with water, calcined, and
- C: ]0 Z5 M7 d, X9 l7 E4 Dmicronized.
( n% A D/ S" NIn the chloride process, chlorine gas is reacted with a titaniumcontaining
$ |- i; v2 b/ ]mineral under reducing conditions to form anhydrous
( `0 |- i9 k1 J7 `0 ntitanium tetrachloride, which is subsequently purified and converted to3 I; \0 f% N5 ?/ j; x
titanium dioxide either by direct thermal oxidation or by reaction with
. \6 N% w$ E! J4 k4 rsteam in the vapour phase. Alternatively, concentrated hydrochloric# }3 o5 F% U$ C% K
acid can be reacted with the titanium-containing mineral to form a
# ~: [6 {$ G7 X/ l( vsolution of titanium tetrachloride, which is then further purified and
9 v9 d+ Q0 D6 ], x% ~converted to titanium dioxide by hydrolysis. The titanium dioxide is
7 |: O9 l Z. A0 x( o; q- K) ffiltered, washed, and calcined.
# b8 |5 M3 f" i2 {" pCommercial titanium dioxide may be coated with small amounts of
3 G2 U4 i; B! g) }0 [alumina and/or silica to improve the technological properties of the' H9 G" T# x# X6 J
product.
3 y" E5 `, f; S, o6 z! E- @C.A.S. number 13463-67-7
8 {: V( Z- A H) m5 JChemical formula TiO2
: D; ~, L% w9 C" ZFormula weight8 q1 `: j( i( s& {
79.88
/ H- j" N, Q! G9 |+ r sAssay9 {7 Z8 G+ U: U$ \
Not less than 99.0% on the dried basis (on an aluminium oxide and. ?" W. K- z" m4 S6 @( \
silicon dioxide-free basis)
0 C2 L: J! M0 w7 a2 bDESCRIPTION
8 e7 @8 W8 f7 B: A H: y! j8 }White to slightly coloured powder1 t: V6 j+ A: f
FUNCTIONAL USES; ~9 ?9 I9 N e$ D2 s6 m+ Z2 H6 x
Colour
" E0 k) L' L8 OCHARACTERISTICS6 R/ X% p( ~0 W% j1 v5 n
IDENTIFICATION
. U, N4 d3 s7 aSolubility (Vol. 4)3 I& |" t, w/ |; A2 e
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
. W/ c, D$ x+ X# N; nsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
0 p6 d3 V7 I. z4 m4 E5 d* _2 Rsulfuric acid.
9 ~9 K( }) T8 T( E. [" ZColour reaction
8 l3 i. T- [3 G% U8 @# ^( d5 yAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of O3 ~0 t+ [4 b. _
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with7 u& ^! h0 ~+ Q" J- }# ~' }$ n
water and filter. To 5 ml of this clear filtrate, add a few drops of
" O6 I- a+ Z6 E# thydrogen peroxide; an orange-red colour appears immediately.
3 W8 I+ R4 Q4 o/ H) sPURITY
. g9 D3 J0 f7 lLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)1 O! \3 d+ \: N) u
Loss on ignition (Vol. 4)$ r( c7 d9 o; g' ?" L8 m$ V. G% `
Not more than 1.0% (800o) on the dried basis- U, X- ^4 Z* x# A% L b
Aluminium oxide and/or% ?9 d( q# V/ I4 u- Q4 q7 f, y
silicon dioxide
/ K# H& t6 O9 RNot more than 2%, either singly or combined) `( |5 Z8 Q5 R' X, d& E; C
See descriptions under TESTS
+ o; B: z7 R" a7 b0 l: SAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
$ \0 U' g, E6 a$ Y& w+ R" q* Zalumina or silica.; O% n3 `* S9 h! d% O* B, @1 b
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
1 H5 V4 n) d h2 m3 Pplace on a steam bath for 30 min with occasional stirring. Filter, ?' X/ w0 @2 J) a) {
through a Gooch crucible fitted with a glass fibre filter paper. Wash
( \( @: u8 ^: p; @. l/ }- C" Zwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the0 ^1 ?- S& T- u) A3 Y v
combined filtrate and washings to dryness, and ignite at a dull red& ~4 Z$ V/ z2 j; K y1 o- J
heat to constant weight.7 `, ~* f1 {% ~: H3 x) d# V1 e
Water-soluble matter
! M. ^) _6 l% d) P! [+ y(Vol. 4)& k% T X( s! |. u0 x
Not more than 0.5%
`% C# @7 t( H* W8 g% qProceed as directed under acid-soluble substances (above), using5 T6 Z6 g& l F# }/ {
water in place of 0.5 N hydrochloric acid." v s$ n6 b T- A: h
Impurities soluble in 0.5 N
! E- _1 m/ }/ k. p( U) v( [hydrochloric acid1 x: a4 Z0 k* k5 h% c G
Antimony Not more than 2 mg/kg% x8 [3 W. `7 q/ H# P/ d
See description under TESTS
8 Z! i9 u' U% g/ TArsenic Not more than 1 mg/kg
# z8 y8 @6 B `9 sSee description under TESTS
8 F) r% A1 n" a2 c+ P3 M3 ICadmium Not more than 1 mg/kg( j( v2 Z J8 M$ E6 @4 w0 {7 }
See description under TESTS5 z$ G/ _# H8 U6 l3 k
Lead
5 y$ q4 ` q4 wNot more than 10 mg/kg
$ G! w# ]- z# I5 X( {, p6 zSee description under TESTS
7 h& \) I! F" xMercury (Vol. 4) Not more than 1 mg/kg6 t0 U2 l6 c! O! x8 X, w" G
Determine using the cold vapour atomic absorption technique. Select a- P: O; v- \' G& Y
sample size appropriate to the specified level+ A$ G0 J' N) ~: u* N8 e* k
TESTS% U$ @7 L2 U6 P& `: ?
PURITY TESTS' T, \3 ]% ^6 G8 e7 l- K, Q
Impurities soluble in 0.5 N
2 s, L' d2 ]3 `; j0 t8 Jhydrochloric acid' f' I4 E. s- @4 Y
Antimony, arsenic,6 E1 u$ j- P; k; h, W
cadmium and lead
2 t4 m8 e; x$ c" p5 n' \/ \(Vol.4)
" V5 u1 h4 F0 W+ d' MTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
6 @& f+ k4 M* g3 Jhydrochloric acid, cover with a watch glass, and heat to boiling on a
9 l8 I2 j9 B1 nhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml' K2 a' ~# c, w8 `8 a v( a
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved' b: @& j6 d' O1 m6 u
material settles. Decant the supernatant extract through a Whatman- B5 U; l; U1 a) u& R
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml/ g; @ ^, S4 f5 p/ Z& T
volumetric flask and retaining as much as possible of the undissolved
* R/ L& }1 G/ lmaterial in the centrifuge bottle. Add 10 ml of hot water to the original/ [, k! [4 i4 M- C6 ^2 }5 u+ o
beaker, washing off the watch glass with the water, and pour the5 ?5 ?. Z& Q6 a* b
contents into the centrifuge bottle. Form a slurry, using a glass stirring* Y0 J( \& V4 f' Z# V4 J
rod, and centrifuge. Decant through the same filter paper, and collect
3 h$ s: c1 Y; s9 Ythe washings in the volumetric flask containing the initial extract.: o: B# q' E. A9 G% X+ A
Repeat the entire washing process two more times. Finally, wash the9 y2 ^- K4 f; |6 J) w
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
+ }5 P6 D( s0 a8 T, oto room temperature, dilute to volume with water, and mix. n5 _3 X: r( _3 a: M+ {9 x
Determine antimony, cadmium, and lead using an AAS/ICP-AES
! `9 i. j# i( j) z- R/ gtechnique appropriate to the specified level. Determine arsenic using the3 h% g# p) V) z" m4 z
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
2 ~6 Y7 }1 I. r7 ~" a! PMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
! Y7 g- h( s+ B2 K1 g. The selection of sample size and method of sample preparation
3 g; O5 w- p0 D4 @# K! q! w; vmay be based on the principles of the methods described in Volume 4.
j4 B8 h% T0 F9 h4 OAluminium oxide Reagents and sample solutions! O6 [5 a Y* m# q% `- S' T2 b
0.01 N Zinc Sulfate0 w) I. h' l- Y8 R1 f0 m/ L$ l; v
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
9 L: @" ~2 z1 Bmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
% n& w+ {/ Z8 N- G3 Oof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of2 }( t* H/ t& Z5 J- n
concentrated hydrochloric acid, heating gently to effect solution, then( X9 |% |; A- L6 G! D. _
transfer the solution into a 1000-ml volumetric flask, dilute to volume4 |: [! @' u0 `* k7 a
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5004 s! L+ A$ D+ q! X1 h
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
# K- }# n- ^1 n3 lconcentrated hydrochloric acid, add 1 drop of methyl orange TS and3 L, [0 P; f6 D. o5 Y1 x9 Q- ?
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
$ v) N- e( f5 P% I- ?# l" X) x' ?$ `dropwise, ammonia solution (1 in 5) until the colour is just completely2 ~2 F# ]# W1 W3 K4 W0 [, M
changed from red to orange-yellow. Then, add:' E: h" a5 M* D. }5 x. `& O% D! O u* m+ F
(a): 10 ml of ammonium acetate buffer solution (77 g of
, J. w7 k. e% rammonium acetate plus 10 ml of glacial acetic acid, dilute to' Y6 i+ I* E* X5 V9 w
1000 ml with water) and0 D5 t J" z; k7 E
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
+ E$ Z8 ?8 ^- l! Bof diammonium hydrogen phosphate in 700 ml of water,
: f( M# I& H; [) P+ Z# K3 fadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,/ C( J) R- m% M+ c4 h6 ~! ? Z
then dilute to 1000 ml with water).& g* S/ Z$ V$ }3 u! \" B- R
Boil the solution for 5 min, cool it quickly to room temperature in a5 r2 m; ^9 [" z8 t$ v1 }4 R
stream of running water, add 3 drops of xylenol orange TS, and mix.0 s1 h% _. V+ a: e
Using the zinc sulfate solution as titrant, titrate the solution to the first2 D* y7 n" a2 `' n7 |6 s+ j3 I+ n
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
8 |6 R0 {$ C2 W5 W& CThis titration should be performed quickly near the end-point by
" k' ~+ A. j" e! W3 Vadding rapidly 0.2 ml increments of the titrant until the first colour
! x3 s9 G; b2 `( }" schange occurs; although the colour will fade in 5-10 sec, it is the true
0 X+ q6 X; c5 Uend-point. Failure to observe the first colour change will result in an+ O+ W+ X# J# o) J4 m. E
incorrect titration. The fading end-point does not occur at the second0 [2 x3 ^. ~; A4 a
end-point.)
7 ~) u# s' W' s( hAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a2 _" ~& t- G9 w o
stream of running water. Titrate this solution, using the zinc sulfate/ B3 ?/ p3 I$ n5 h
solution as titrant, to the same fugitive yellow-brown or pink end-point r/ d+ L' `& Y4 u& X7 {( w
as described above., |+ x" I. Q* N+ J! O; D
Calculate the titre T of zinc sulfate solution by the formula:
' }2 l. Z( i1 A/ b( yT = 18.896 W / V
* j" G/ w: n7 h7 awhere
6 {, ?) @& B$ y. g vT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
; h. N L& E* A5 G6 x* N; OW is the mass (g) of aluminium wire% `' F& s. p4 [0 u1 s$ S
V is the ml of the zinc sulfate solution consumed in the
9 [ u9 P4 {, k; dsecond titration, R$ U9 L( c) }5 W+ B
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and; W- |2 d2 ~, T- z) n# e* ^
R is the ratio of the formula weight of aluminium oxide to! ~: O' k2 j! u
that of elemental aluminium.
& f! ~8 Q6 x% _Sample Solution A( _ ] ]5 |7 R: I
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
2 h0 A( J4 Q( D5 {$ lglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
( M H& D! q1 S& ]% |4 \' Y(Note: Do not use more sodium bisulfate than specified, as an excess8 A6 r5 n& q- f) l- u8 R
concentration of salt will interfere with the EDTA titration later on in the$ I( e* M% P+ ?! R. h* _
procedure.) Begin heating the flask at low heat on a hot plate, and
, d/ F! `( X; R. Pthen gradually raise the temperature until full heat is reached.. I, u0 I- |4 J+ e( f3 p( y
(Caution: perform this procedure in a well ventilated area. ) When. u5 T& T0 ]& f! ^4 `
spattering has stopped and light fumes of SO3 appear, heat in the full
) N$ t2 `7 q' M, Q5 u/ l9 |flame of a Meeker burner, with the flask tilted so that the fusion of the7 m% U& D6 B* b j3 O
sample and sodium bisulfate is concentrated at one end of the flask.
5 M+ k& P( `4 B8 E/ r/ \- ?7 m+ TSwirl constantly until the melt is clear (except for silica content), but
/ @5 `' \+ Y3 h2 V# Z8 k( l; T1 y+ _: Lguard against prolonged heating to avoid precipitation of titanium2 [% R/ I* U i: t9 a \9 k
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until( f# R4 o- W X; W( A
the mass has dissolved and a clear solution results. Cool, and dilute to
. q4 `0 u0 P# b( {0 g' J/ U$ K120 ml with water. Introduce a magnetic stir bar into the flask.2 v8 E+ H: N0 p9 s; f4 K* b
Sample Solution B
* Q* z+ L, @( ~$ F1 C! g) K2 dPrepare 200 ml of an approximately 6.25 M solution of sodium( R/ O/ N, ~4 ]' @0 [2 J
hydroxide. Add 65 ml of this solution to Sample Solution A, while
" d+ B& [: n a! N3 }2 C. [stirring with the magnetic stirrer; pour the remaining 135 ml of the6 E7 U5 D9 S1 G1 a* t0 @
alkali solution into a 500-ml volumetric flask.7 D/ H5 ]7 }# P
Slowly, with constant stirring, add the sample mixture to the alkali
E! R( [, B; n3 A7 }( D9 hsolution in the 500-ml volumetric flask; dilute to volume with water,& V$ z1 l2 I. y2 h/ n' o" N
and mix. (Note: If the procedure is delayed at this point for more than+ r. L& F5 e- [+ \
2 hours, store the contents of the volumetric flask in a polyethylene
! j; W$ h+ c( h Nbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
1 @% l- S% d0 Z" f/ V+ Lthen filter the supernatant liquid through a very fine filter paper. Label
' h8 O" V+ [+ a# P1 j Bthe filtrate Sample Solution B.! i( x! j7 O( ]: n6 m9 S" q9 g% C
Sample Solution C
7 f* E2 _3 k. u4 T6 WTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
+ ^2 ~/ b5 {* c( A$ dflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
: p @0 w; P1 `, X' h0 U3 Ysolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02/ I" g8 p7 X4 a! N; f/ W( v! S% E
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
3 U0 Q7 }* p% e2 C" K5 t0 {known, calculate the optimum volume of EDTA solution to be added9 w! S4 I2 R4 |0 B
by the formula: (4 x % Al2O3) + 5.]2 m9 p- }$ M: `, C& l
Add, dropwise, ammonia solution (1 in 5) until the colour is just
9 o6 [- @7 k2 ?3 q+ g" v. Ocompletely changed from red to orange-yellow. Then add10 ml each- ], J1 c' b- v! ]: ]8 }! D! X, e
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
/ N: l, @+ d& D) k4 H2 |8 x3 g& Droom temperature in a stream of running water, add 3 drops of xylenol8 {0 C7 u q8 x; Z: t3 b
orange TS, and mix. If the solution is purple, yellow-brown, or pink,0 y* B% l; a. r. x6 k& R
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired1 M( p' k+ v9 V7 [
pH, a pink colour indicates that not enough of the EDTA solution has7 t- ~9 {. S0 L/ r
been added, in which case, discard the solution and repeat this5 c, H# F6 y N w
procedure with another 100 ml of Sample Solution B, using 50 ml,. z0 M: c' t" h$ N2 g
rather than 25 ml, of 0.02 M disodium EDTA.0 A; W2 f7 [/ a' N2 g1 p4 p7 g3 u. X; x( E
Procedure
4 V1 v) i% S2 n2 QUsing the standardized zinc sulfate solution as titrant, titrate Sample
! k3 \0 Q& E. P: i" FSolution C to the first yellow-brown or pink end-point that persists for
+ P8 j1 T/ X! L7 X+ |, m1 ]5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
( t8 W9 D( l, m, P4 q/ N- `titration should require more than 8 ml of titrant, but for more accurate
" x3 d# b; ^& q% h0 |+ xwork a titration of 10-15 ml is desirable.
+ d! X e2 v9 ` k" s- N+ {& c/ ?Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5 q: }1 f4 m$ C# k
min, and cool in a stream of running water. Titrate this solution, using
# U& V, A7 |5 Fthe standardized zinc sulfate solution as titrant, to the same fugitive
9 v- e4 a8 a/ p$ Byellow-brown or pink end-point as described above.
" r0 h' @/ ^' @" M+ B9 _* E# [Calculation: p A# D/ l' A0 R; d
Calculate the percentage of aluminium oxide (Al2O3) in the sample
: u/ `2 U- F* \! ~3 Ktaken by the formula:8 q8 p: f6 m) C- H2 L3 P
% Al2O3 = 100 × (0.005VT)/S
g6 Q" h* E( T+ c8 F zwhere
' J3 t; u" w6 ^& O) AV is the number of ml of 0.01 N zinc sulfate consumed in
+ u1 {8 M7 \3 s/ D9 pthe second titration,
5 X# N' O5 B7 }5 k' m0 M( nT is the titre of the zinc sulfate solution,& g& {8 e, z( I* W6 U! E7 |6 n9 \
S is the mass (g) of the sample taken, and
7 R2 j& {) U) e7 p8 s0.005 = 500 ml / (1000mg/g × 100 ml).6 M8 V3 D, H- U7 K
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica. X2 P5 i; u8 _9 R1 Z5 G8 d
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).; d1 z! O! x9 x& a& X+ j% I
Heat gently over a Meeker burner, while swirling the flask, until2 \( a; a2 N y7 O# i3 @3 N
decomposition and fusion are complete and the melt is clear, except' D. x2 G5 a q- y
for the silica content, and then cool. (Caution: Do not overheat the/ v5 }& |& u, [& G P
contents of the flask at the beginning, and heat cautiously during, {) N" X1 C0 f( W, q( T% G; N
fusion to avoid spattering.)
. Q1 e& ?: T) ], v+ S+ i. F. cTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat3 K4 V8 _* l# s8 V7 v' o, \* r
carefully and slowly until the melt is dissolved. Cool, and carefully add, w$ L% k4 l. S# D
150 ml of water by pouring very small portions down the sides of the
s6 K/ L5 d/ ~7 S6 z+ {: fflask, with frequent swirling to avoid over-heating and spattering. Allow# g) U$ M9 p: T8 S; o
the contents of the flask to cool, and filter through fine ashless filter9 l" v3 V* F' ^" x& z2 ?1 [* K
paper, using a 60 degree gravity funnel. Rinse out all the silica from
6 M. z. W" C K2 I0 W! S6 X% Mthe flask onto the filter paper with sulfuric acid solution (1 in 10).' y4 z: u! |4 z) {/ T
Transfer the filter paper and its contents into a platinum crucible, dry in
% a6 W& L- v' I+ C8 [; ban oven at 1200, and heat the partly covered crucible over a Bunsen
' s. l; g/ V4 `% Zburner. To prevent flaming of the filter paper, first heat the cover from
$ |! V, c2 ^! R0 D; a* o7 h/ rabove, and then the crucible from below.
$ w$ ]8 F# e9 @( m9 j- EWhen the filter paper is consumed, transfer the crucible to a muffle( b, H6 y& B' \/ d1 }* m4 u
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
) @) D' ^3 O: b' Uweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
. y) p( v# K' ~' H# Y9 Ahydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first9 Q& R9 y& _6 t6 d% o
on a low-heat hot plate (to remove the HF) and then over a Bunsen
) H: p6 X _4 k1 {) n& D& q4 [% ^+ Eburner (to remove the H2SO4). Take precautions to avoid spattering,+ e( r( @$ z! ~" [; Z! `- O4 Q
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
4 p% Z- p @. D1 tdesiccator, and weigh again. Record the difference between the two8 @5 A; b1 @9 B: U" n7 _+ K$ x
weights as the content of SiO2 in the sample.7 e) A+ p9 t0 x' Q% h
METHOD OF ASSAY8 u, ?4 \$ L. A/ s
Accurately weigh about 150 mg of the sample, previously dried at 105o
' |+ S2 ] F0 E. s' g: Dfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
% J3 i. A& R6 v4 ?and shake until a homogeneous, milky suspension is obtained. Add 30
% y0 B+ v. K G2 P/ Z9 Mml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially; ^0 @/ ]$ V# M! f: M+ p
heat gently, then heat strongly until a clear solution is obtained. Cool,* E# D' ~1 f6 n: n) J
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric7 W# p m; z% Y, w: d" [6 M' D
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
! s% J5 x2 o& ]1 I" D! W: ?rubber stopper fitted with a U-shaped glass tube while immersing the
$ I& Z; V) R! Y( B% k$ r( Eother end of the U-tube into a saturated solution of sodium
4 E% y& u7 Z% v, ]bicarbonate contained in a 500-ml wide-mouth bottle, and generate
+ q, y7 l7 c! ^! H3 shydrogen. Allow to stand for a few minutes after the aluminium metal/ S7 z) I6 x( t+ ^, F) s* t
has dissolved completely to produce a transparent purple solution.
- V6 K' z" q, }1 H, F& y" q) H+ ~Cool to below 50o in running water, and remove the rubber stopper' D6 x" i9 E: v6 X Y6 O2 @9 w+ _
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate2 `: b5 r- K; H% n
solution as an indicator, and immediately titrate with 0.2 N ferric
; @% L2 F- @! ]: V, cammonium sulfate until a faint brown colour that persists for 30
9 O7 q) D3 Q( J" y5 Z3 x4 sseconds is obtained. Perform a blank determination and make any
! q' ? ^5 r! \1 g- ^. O$ xnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is3 y! {9 J% l g, K
equivalent to 7.990 mg of TiO2.
" i2 b' N% \. A( \' |; {+ X |
|