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二氧化钛(钛白粉)
二氧化钛(钛白粉)9 H8 z( |0 B/ y' V7 N3 z' _& w
0 A; J& m) c- }% v, J# {6 WJECFA关于二氧化钛(钛白粉)的结论, M8 A2 O* V' U' i6 m- v _. k
( n# ~6 }2 g& H. _
摘要: 2006年JECFA关于二氧化钛的结论
# o& G* O2 ]9 S, @ADI值:不作限制。/ X5 C' q& r! d5 f N7 k
功能:着色剂
* f- ^& w; y* }: e' v6 d( M8 ^
+ V' D$ Y2 R0 Q, n( rTITANIUM DIOXIDE
0 ?# |6 }, z& m* h, Z+ b% h; yPrepared at the 67th JECFA (2006) and published in FAO JECFA
- g5 I- p' a' }* y; @! t6 YMonographs 3 (2006), superseding specifications prepared at the 63rd
7 f, V# _: m, H1 h& m# Z* nJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
; h0 t4 e) U$ p4 Y& o \5 u, f8 QCombined Compendium of Food Additive Specifications, FAO JECFA; R3 h) J5 U3 [9 e
Monographs 1 (2005). An ADI “not limited” was established at the 13th
# }4 n4 t X' Z( P+ D' j6 A: YJECFA (1969).; O" ^2 F5 Z; d' V' F! C! Z" e, x7 t4 ^
SYNONYMS9 E$ ?9 j3 X. q/ [: p
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171 u7 @7 W" \9 R5 V
DEFINITION% }' v) v8 g: c3 K/ d" o
Titanium dioxide is produced by either the sulfate or the chloride
7 b1 L6 \4 i+ q, Z/ J3 Dprocess. Processing conditions determine the form (anatase or rutile) b) P5 U& J8 q; E4 a" y" h
structure) of the final product.
& J! d/ t; h% D3 u$ [# ^$ l. M4 Z8 JIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
4 E7 Y( A8 ?1 ~% n/ Uor ilmenite and titanium slag. After a series of purification steps, the
: _( A9 U, i9 [6 l4 f! ?, j, i1 h0 Lisolated titanium dioxide is finally washed with water, calcined, and& t% i5 a( m( m/ P
micronized.
1 }* V7 f2 R+ w& D( ~' I. U& V# C6 IIn the chloride process, chlorine gas is reacted with a titaniumcontaining
3 T6 y9 Z& ]* t: Emineral under reducing conditions to form anhydrous
8 S/ r: M+ D9 H' xtitanium tetrachloride, which is subsequently purified and converted to9 N8 N; G" g! X4 g
titanium dioxide either by direct thermal oxidation or by reaction with: z( J+ {" t4 E( ?; w( L- G
steam in the vapour phase. Alternatively, concentrated hydrochloric
: v, ~- C* Z+ P lacid can be reacted with the titanium-containing mineral to form a
: q% B2 o' w) D; |solution of titanium tetrachloride, which is then further purified and% k- @9 a* I( a# ~" e4 y+ K) v$ p
converted to titanium dioxide by hydrolysis. The titanium dioxide is
- h) t% L1 ], W! `filtered, washed, and calcined.2 T2 H2 G3 X, Z1 [/ N' o
Commercial titanium dioxide may be coated with small amounts of( w/ m9 A+ ^1 X0 f, {
alumina and/or silica to improve the technological properties of the
& ?3 [. V" U" q0 oproduct.
9 s! x6 r4 s! h/ U iC.A.S. number 13463-67-7
2 `# g" C5 N/ K% lChemical formula TiO25 ^; b) h0 \7 `# M2 `% ?
Formula weight" ?; X/ o+ X2 ]6 C; D, `6 c
79.88
% j0 u- H. H( _2 N2 v" h9 Q- oAssay
# ~4 \8 o' v5 aNot less than 99.0% on the dried basis (on an aluminium oxide and
5 Q: U6 c/ P+ f$ K' {; dsilicon dioxide-free basis)# U( K% Z# _+ W# U3 {* L
DESCRIPTION |3 O) M" u* Z P( ^8 s: _
White to slightly coloured powder5 D' E% X( Y& {- ~
FUNCTIONAL USES
+ a) ~) |; O7 R6 f9 b, f' @Colour6 g/ [+ T- T1 F: S
CHARACTERISTICS
0 c4 E+ w* q2 A$ h( H- b3 uIDENTIFICATION
. X( X! I& K( C& T8 }- M9 LSolubility (Vol. 4)/ w0 m, s. U1 B' ^
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic" t8 _0 j; R( X5 W: L; i) R, i
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
5 U4 V T2 O% ~2 t: P9 \sulfuric acid.
% m0 ~" F/ ^8 CColour reaction+ l8 X8 L" j7 l7 M% P4 n
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
$ H: p, J8 C/ }sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
6 t, I! ^) l* l$ w% c3 Kwater and filter. To 5 ml of this clear filtrate, add a few drops of
* O5 x5 u1 U, h9 ^* bhydrogen peroxide; an orange-red colour appears immediately.
8 P' W% b+ n& P" j3 u! mPURITY1 \' w: p; C& x2 x0 I& w# N
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
( `9 A9 ~/ G7 P8 X6 {- y9 pLoss on ignition (Vol. 4)
" d) p9 x; _( o' N7 cNot more than 1.0% (800o) on the dried basis
% L Z3 P& Z* T/ h2 SAluminium oxide and/or- q! Z6 ~2 c5 ^! H5 v
silicon dioxide/ {3 E% U, H2 g
Not more than 2%, either singly or combined
- n( C9 ]) ?$ c" HSee descriptions under TESTS5 o# v8 ]( T- C) {% y1 _# d) [
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing) h( U2 R6 Z. y
alumina or silica.: g3 n" O5 l5 M$ V) K2 R
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and1 U0 H! W, E/ O) Z T/ h O3 ~; G
place on a steam bath for 30 min with occasional stirring. Filter
( F1 p3 O6 O5 I7 c: f) _through a Gooch crucible fitted with a glass fibre filter paper. Wash
6 Z: W. U, h; m+ a6 Z: B9 \% Nwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
5 v" S/ G2 G" F; b0 V1 @, fcombined filtrate and washings to dryness, and ignite at a dull red% y4 l1 S, u. E+ V
heat to constant weight.
, _$ Q* B2 D0 o7 d; e6 e, i4 o' bWater-soluble matter7 v" g4 m& [$ S- H. J: D
(Vol. 4)9 K T2 b0 \6 F. s0 Y, z7 u, {
Not more than 0.5%
0 W0 f' j- Q1 l: h% i5 y7 `Proceed as directed under acid-soluble substances (above), using
0 V, N- v2 R, R: Lwater in place of 0.5 N hydrochloric acid.$ E* q3 W( k5 {; U7 n( w6 j) H) i3 n
Impurities soluble in 0.5 N
6 X. w8 n2 Q- o( m) Z- r9 ^hydrochloric acid
& P& ~2 |# L! BAntimony Not more than 2 mg/kg" i9 N/ f9 d C+ y* |+ ?9 R
See description under TESTS
$ u+ `( _/ i( O& ~6 I9 gArsenic Not more than 1 mg/kg
- Y! J, ]( d: [3 pSee description under TESTS
! R2 X5 v. h9 \% P- Z- S- T8 Z8 RCadmium Not more than 1 mg/kg
1 X2 G# B7 B$ O: Y0 _* [ bSee description under TESTS
7 N3 l% `$ c* q6 P0 m% d1 }Lead
( T. B3 J- {) `Not more than 10 mg/kg4 @' o% `( a3 E9 E
See description under TESTS
4 B$ b* n5 a7 {Mercury (Vol. 4) Not more than 1 mg/kg
1 k e) m* }4 A6 S" rDetermine using the cold vapour atomic absorption technique. Select a: ?+ z! |1 c8 }7 E$ ~, s
sample size appropriate to the specified level2 ]! `, A& m* X1 L6 G' ~( x' X
TESTS M9 o' z- I% q3 n, L
PURITY TESTS
/ F4 p z/ \& L, I6 f m# e6 ?Impurities soluble in 0.5 N8 }$ A. A3 |* |% N8 s8 g
hydrochloric acid
9 t6 T# B+ G) \* g, k* ]Antimony, arsenic,9 J7 v2 y$ q5 @
cadmium and lead
" i; T D$ @( {% a(Vol.4)
8 _' e) x% a. F$ H; xTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
6 {( u* G) r' z. ohydrochloric acid, cover with a watch glass, and heat to boiling on a
0 G; l+ J F8 X0 Vhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml/ c% s6 R! t" J/ Y1 x$ H
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
6 i; k1 K/ c" N7 x0 Bmaterial settles. Decant the supernatant extract through a Whatman
4 _7 u, h8 N" p1 s8 w) V+ PNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml0 Q3 r0 j; V4 K- R
volumetric flask and retaining as much as possible of the undissolved
+ D0 \( V9 p d7 V: P# z1 p: gmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
9 }. {7 i/ ` K( Z; U; ebeaker, washing off the watch glass with the water, and pour the5 L, y/ |/ ]/ [
contents into the centrifuge bottle. Form a slurry, using a glass stirring
* ^* l4 q; D# m- [+ g; u# Arod, and centrifuge. Decant through the same filter paper, and collect2 e j* k7 Y4 k( }- x' @
the washings in the volumetric flask containing the initial extract.* n0 Q9 @% O3 z4 w m9 c
Repeat the entire washing process two more times. Finally, wash the
6 j, \8 m$ e# E! g$ A. Lfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask2 N5 q: |! [: Q# i( i
to room temperature, dilute to volume with water, and mix.
, w. e- }* }6 I0 zDetermine antimony, cadmium, and lead using an AAS/ICP-AES, j1 O5 `" j7 D! S. U) D0 E7 v8 o
technique appropriate to the specified level. Determine arsenic using the4 h, t4 ?0 c" ? x
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
2 P" o) d. Q, B6 T3 K1 `Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
k; V- M/ R+ y5 o6 ?# Y% H/ _; g1 g. The selection of sample size and method of sample preparation7 }1 U3 J+ A! t& e t
may be based on the principles of the methods described in Volume 4.
% q6 J& h: Z+ H1 ?) Z' D8 ?; ZAluminium oxide Reagents and sample solutions9 l2 @& q; G7 @1 U0 O j
0.01 N Zinc Sulfate
# S6 ]& G, T9 RDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
9 f5 m4 O) f9 J! M0 T* ^1 X6 Gmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg) R0 }4 r2 t8 |( I2 X( t
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
, ^+ Z. ~* x, ], `. ^& \$ uconcentrated hydrochloric acid, heating gently to effect solution, then3 Y3 l% A' r3 ?% Y: x# s% V3 P7 e
transfer the solution into a 1000-ml volumetric flask, dilute to volume0 H# K6 o+ |3 R& g8 a
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5002 j9 n C9 b' l# b" d& s0 B
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
- R+ l* X J7 O( p9 t% j/ V3 pconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
: x: @" K! C7 ~* j. |) ]/ L25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
0 F) f4 g7 m7 b) H' s; adropwise, ammonia solution (1 in 5) until the colour is just completely
! h) O' o L9 @4 o( E' H) Vchanged from red to orange-yellow. Then, add:
a( d! \5 S# O! W! U% [* l(a): 10 ml of ammonium acetate buffer solution (77 g of
0 ~' c* {' c6 N' @9 i+ B5 D+ S Eammonium acetate plus 10 ml of glacial acetic acid, dilute to
7 P- D7 c7 g K) `' i, L7 h* e1000 ml with water) and
: v1 @/ [' {; D C2 J* D(b): 10 ml of diammonium hydrogen phosphate solution (150 g
. `3 X$ V9 m9 }of diammonium hydrogen phosphate in 700 ml of water,( b9 M/ B X) r; }% n
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,& [) N# H- |: |% e' O
then dilute to 1000 ml with water).
5 `3 L- g( ]* p9 E/ M o( QBoil the solution for 5 min, cool it quickly to room temperature in a
. M' H; U5 f' k! N+ b E( F& ^7 ustream of running water, add 3 drops of xylenol orange TS, and mix.
8 \. F( v) @: |5 _ AUsing the zinc sulfate solution as titrant, titrate the solution to the first4 J7 W. e2 E" T$ Y/ V2 i
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
" P7 i: R, U# l+ V9 NThis titration should be performed quickly near the end-point by3 S. s7 Z2 ~, J9 L" ~& F
adding rapidly 0.2 ml increments of the titrant until the first colour* l! ?& \' S/ z( q0 V3 `
change occurs; although the colour will fade in 5-10 sec, it is the true
& ?3 R+ x' u0 e4 X: R7 Cend-point. Failure to observe the first colour change will result in an
+ m% \& d) K! R# l1 r0 h/ V+ Yincorrect titration. The fading end-point does not occur at the second8 B% N- n; h& c7 c: k3 K( o4 R
end-point.)! s7 t0 x3 y1 u, p6 F
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a! G) L- i% r" P* p* E9 q& B
stream of running water. Titrate this solution, using the zinc sulfate% D9 x0 o G; f7 U
solution as titrant, to the same fugitive yellow-brown or pink end-point
& X) T" U s5 a2 Kas described above.; }; U, g! r0 X0 j
Calculate the titre T of zinc sulfate solution by the formula:8 c. C1 W, Q! e
T = 18.896 W / V
& @8 |5 L( J8 r# awhere- \' V$ k$ f. _6 y: y
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution- d! t/ I/ O. |' S
W is the mass (g) of aluminium wire! l8 u* n* \% W# N/ G
V is the ml of the zinc sulfate solution consumed in the* W% H# p# }5 i) c
second titration
$ j6 C( h4 N( b- J A18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and: g2 X% J# A& V9 O6 G
R is the ratio of the formula weight of aluminium oxide to+ l6 G$ b! x0 G$ w
that of elemental aluminium.7 u7 ^" _0 \+ ^6 V
Sample Solution A
) _6 u f6 `; u9 CAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
- O' a6 M2 C& Wglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).; i2 J7 d- R. T
(Note: Do not use more sodium bisulfate than specified, as an excess
; v. i' a; r [concentration of salt will interfere with the EDTA titration later on in the+ c7 {8 _* M# L
procedure.) Begin heating the flask at low heat on a hot plate, and8 S t) x) D! }
then gradually raise the temperature until full heat is reached.
3 i; J8 L; B% j Y2 m W4 s) [0 ^% {: e(Caution: perform this procedure in a well ventilated area. ) When; x5 w5 \0 w' W
spattering has stopped and light fumes of SO3 appear, heat in the full" x$ [5 B5 _# V1 B% Q
flame of a Meeker burner, with the flask tilted so that the fusion of the
6 r% y. P' [" b$ u' {3 Csample and sodium bisulfate is concentrated at one end of the flask.
; b q9 y0 D. H1 rSwirl constantly until the melt is clear (except for silica content), but. s9 T8 n y# |/ Q6 p7 H" f, {+ ~2 z
guard against prolonged heating to avoid precipitation of titanium
( N) a8 Z3 o0 y" j |9 Mdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until C0 g+ J4 s( |* P
the mass has dissolved and a clear solution results. Cool, and dilute to# R( E9 t- B1 c* x$ d) y, f
120 ml with water. Introduce a magnetic stir bar into the flask.
5 w0 o" O6 h0 F4 I7 G* }( E) ~Sample Solution B
9 n( B3 J5 R; d" CPrepare 200 ml of an approximately 6.25 M solution of sodium! t- r e: J' |
hydroxide. Add 65 ml of this solution to Sample Solution A, while" n2 M, {8 ~9 l1 r8 s. \
stirring with the magnetic stirrer; pour the remaining 135 ml of the
4 d! S) z! A! {9 p3 Z- w* E4 P5 Aalkali solution into a 500-ml volumetric flask.# e( B# u5 V7 v+ r7 x% a% a# }* I% r
Slowly, with constant stirring, add the sample mixture to the alkali
; ?0 L9 U2 D8 Y7 U3 Hsolution in the 500-ml volumetric flask; dilute to volume with water,, ?5 f* J, J @) X. v0 h2 ]2 G
and mix. (Note: If the procedure is delayed at this point for more than
0 {( ?" {7 D: o2 d1 [5 O- K c) N2 hours, store the contents of the volumetric flask in a polyethylene
1 Y: v& M+ m) V7 E! _9 Ybottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
1 c6 ]) x- z& O$ w lthen filter the supernatant liquid through a very fine filter paper. Label
2 ~6 e& @* J' b' y4 Xthe filtrate Sample Solution B.
# m/ e' l# ~) `Sample Solution C
# g% x: ^# w# z; Y3 y' NTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
: L2 E0 m1 d6 }! G- pflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
+ G" l; U" I1 C! T( z6 Qsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.026 _& l$ A" v% Z" a
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
4 g" Q( x2 L* eknown, calculate the optimum volume of EDTA solution to be added
, v7 C2 P% S, u$ N4 O0 H' kby the formula: (4 x % Al2O3) + 5.]
5 s J+ Y( e1 M+ N% d7 `% M: v* wAdd, dropwise, ammonia solution (1 in 5) until the colour is just
/ c& B* V6 ?/ a" ucompletely changed from red to orange-yellow. Then add10 ml each5 a1 d& x# w6 A8 {
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to& _) B, Y8 j, l& g* w
room temperature in a stream of running water, add 3 drops of xylenol' q6 ?2 y' B# T; y9 M+ _; m
orange TS, and mix. If the solution is purple, yellow-brown, or pink,1 I7 Q# V' C8 ~; i. P
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
" ^. g2 I" e. ?% RpH, a pink colour indicates that not enough of the EDTA solution has, j- s+ B: g% ]+ A
been added, in which case, discard the solution and repeat this0 z7 H7 i7 Z" \% ?/ P
procedure with another 100 ml of Sample Solution B, using 50 ml,
; `' M) t/ C4 z& s: z% arather than 25 ml, of 0.02 M disodium EDTA.0 g. x8 \9 \, ?7 U0 o& X
Procedure
* B% W% }, k! P# S) xUsing the standardized zinc sulfate solution as titrant, titrate Sample4 B* e6 x) k( C* s; J3 D
Solution C to the first yellow-brown or pink end-point that persists for: o' V) f0 s0 V( g3 R
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
5 R( _' z7 J; J8 A- z8 O# \titration should require more than 8 ml of titrant, but for more accurate
, Y+ x8 q& P0 I* k, h% P8 ^work a titration of 10-15 ml is desirable.
' o# S( g. j% C6 A h/ l, j wAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
& d9 A( |+ M$ E: _min, and cool in a stream of running water. Titrate this solution, using
0 m% l0 v' Q) b1 \" i% R u# othe standardized zinc sulfate solution as titrant, to the same fugitive
0 h. J( i# v3 T$ a" T& Uyellow-brown or pink end-point as described above.: K$ v. ^- E/ e" V
Calculation:
* d2 M4 y7 n3 F- V0 k' V+ [Calculate the percentage of aluminium oxide (Al2O3) in the sample' x6 ~4 a6 o5 E4 i
taken by the formula:8 b+ Y! y$ F. @
% Al2O3 = 100 × (0.005VT)/S
" O/ s/ m" f0 i$ Jwhere
3 E& a# I/ C0 }# L8 C) `: z$ AV is the number of ml of 0.01 N zinc sulfate consumed in$ K* {9 w1 R) g" Q9 L+ Y
the second titration,0 k. H( V7 h( S5 M
T is the titre of the zinc sulfate solution,
3 I' p1 U: T; j* r$ nS is the mass (g) of the sample taken, and3 `3 \! n+ C1 `+ z4 I" j
0.005 = 500 ml / (1000mg/g × 100 ml).; I3 P; w! U( W4 d' c1 J
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica! M9 X! O4 M% @1 t6 ~
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
8 i( W' m8 M2 R: j& y1 @/ bHeat gently over a Meeker burner, while swirling the flask, until
5 ]$ f3 v! i2 Z. S( ^$ b3 t( Tdecomposition and fusion are complete and the melt is clear, except8 U* c7 f+ B/ ?9 X0 j. n
for the silica content, and then cool. (Caution: Do not overheat the M8 u8 w; S+ c4 N6 B1 u
contents of the flask at the beginning, and heat cautiously during i" _( a P; [5 x3 t; i
fusion to avoid spattering.)& i1 t! e( O( D' C9 y. U8 C
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
& C- u9 q$ t/ G j1 Ecarefully and slowly until the melt is dissolved. Cool, and carefully add4 D5 ]3 i. A9 V( b: c7 R' c u
150 ml of water by pouring very small portions down the sides of the& V' ~* j9 ^/ s
flask, with frequent swirling to avoid over-heating and spattering. Allow
6 e, W0 K( l6 E& T1 y* B U) }# Athe contents of the flask to cool, and filter through fine ashless filter
/ Y' l1 F4 s6 }, Cpaper, using a 60 degree gravity funnel. Rinse out all the silica from
7 ]0 A0 B$ K7 x; V) h7 q7 ethe flask onto the filter paper with sulfuric acid solution (1 in 10).
- x2 F4 I9 C3 n, x0 _' k6 r1 A6 ?Transfer the filter paper and its contents into a platinum crucible, dry in; a; j0 q3 p" C% {/ O& T* c
an oven at 1200, and heat the partly covered crucible over a Bunsen Y8 w6 N, l+ a& W- n$ [6 q
burner. To prevent flaming of the filter paper, first heat the cover from
. Q4 a6 q- p7 habove, and then the crucible from below.
o" n5 | D( y1 n; F- _; L* cWhen the filter paper is consumed, transfer the crucible to a muffle$ J5 c5 N6 B5 D& {
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and) R; o5 p8 O9 n) s
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated: l# W/ d4 d C: n
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first$ o3 |; j. s2 H5 t# K& Y
on a low-heat hot plate (to remove the HF) and then over a Bunsen
6 z% J/ ~$ D- I& J7 E9 f1 tburner (to remove the H2SO4). Take precautions to avoid spattering,
' z) v' I+ K7 r3 n8 C/ }especially after removal of the HF. Ignite at 1000o for 10 min, cool in a# C c* |0 Z2 u( T+ I. j
desiccator, and weigh again. Record the difference between the two* p; t- y- L& t" A/ E# j! \
weights as the content of SiO2 in the sample.
# U1 R1 K4 T% e* t# V# K3 o+ X; X: vMETHOD OF ASSAY( d( b$ p- ^) V# i4 y9 j% U" F
Accurately weigh about 150 mg of the sample, previously dried at 105o
4 F K/ H8 d/ \0 _. x% n5 ?for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water# J1 _/ j8 ?" N
and shake until a homogeneous, milky suspension is obtained. Add 30
( G; X8 ^4 z3 B5 |ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially% ^% d! Z; G2 R9 ]" A
heat gently, then heat strongly until a clear solution is obtained. Cool,( {. V% t7 v% |& p. h
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
4 ^" E% U- C3 M% t5 oacid, and stir. Add 3 g of aluminium metal, and immediately insert a8 V$ g0 ~* {# U X6 J0 g: n
rubber stopper fitted with a U-shaped glass tube while immersing the
# A# I/ e9 C' L& y( l* x+ P: Zother end of the U-tube into a saturated solution of sodium
: B" u% x8 ~7 l+ Y* u- Gbicarbonate contained in a 500-ml wide-mouth bottle, and generate
: ^0 y$ k) t. E+ x3 G2 Xhydrogen. Allow to stand for a few minutes after the aluminium metal
7 Z/ A2 F+ u& c& ?! y! r" {; [3 Ihas dissolved completely to produce a transparent purple solution.6 U# W) F4 F& E% B& s& h1 P$ R
Cool to below 50o in running water, and remove the rubber stopper
" ]! |/ C' ?2 e1 Q, P& ~1 k8 `carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate$ z& x+ R% T" \
solution as an indicator, and immediately titrate with 0.2 N ferric2 R+ [6 L: t% S! [; e7 E/ E
ammonium sulfate until a faint brown colour that persists for 30
% I0 ~7 }/ Y4 w4 g7 Fseconds is obtained. Perform a blank determination and make any2 P- M. P1 i" W" Q
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
2 Q1 \5 O1 D7 S! |equivalent to 7.990 mg of TiO2." K! o" e- W" J8 d8 [& U* g! L
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