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二氧化钛(钛白粉)
二氧化钛(钛白粉)
% A" m9 q9 f- O* z+ _- F2 ^! P) p, J& A- N s& R6 {7 t& {: |
JECFA关于二氧化钛(钛白粉)的结论5 ]4 J' p" n- V& h
9 t6 }& S7 @+ D/ I3 E# B
摘要: 2006年JECFA关于二氧化钛的结论
8 \& ]; u/ a8 NADI值:不作限制。
9 o# Y- s- Y1 C9 b( l功能:着色剂
& K9 K6 v7 \ N# h% \4 a3 V1 g# B0 e7 J6 b# v* [
TITANIUM DIOXIDE
4 f2 C' K6 |% T9 R2 U+ o9 n. O A/ NPrepared at the 67th JECFA (2006) and published in FAO JECFA( _8 E1 j$ h4 s5 h' `! E0 }. P
Monographs 3 (2006), superseding specifications prepared at the 63rd
! ?3 @; ]4 h& q, q/ QJECFA (2004) and published in FNP 52 Add 12 (2004) and in the% K, L$ M3 c: H1 T5 z2 }5 t
Combined Compendium of Food Additive Specifications, FAO JECFA
+ m5 g) t, G4 ~) l- \+ v7 j hMonographs 1 (2005). An ADI “not limited” was established at the 13th, Q: y+ L8 [; H0 @) ^- V
JECFA (1969).4 Z# O$ H8 g& }* R( j4 O& Q
SYNONYMS
4 e Y5 p0 i/ E0 `2 FTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1713 _' J- p, i" D" W( n2 z4 j
DEFINITION) s/ K' s8 u' A% ?7 `( }
Titanium dioxide is produced by either the sulfate or the chloride/ V8 n% d) W' n- D3 x5 d
process. Processing conditions determine the form (anatase or rutile, O% P* D2 B! S
structure) of the final product.+ ~" j. Z) e" T2 G$ h. \1 |
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)1 N, t& Y; o/ D% U2 x5 D
or ilmenite and titanium slag. After a series of purification steps, the
: P; S8 a j6 l( C& i* Y3 j2 D8 O+ kisolated titanium dioxide is finally washed with water, calcined, and
; v6 ]1 z! \6 e* c2 p% Nmicronized.+ v: G. J- d" W! N% K4 r
In the chloride process, chlorine gas is reacted with a titaniumcontaining
( {7 W7 A# d7 E/ V* }mineral under reducing conditions to form anhydrous$ L4 h* ?8 D# Z |* v$ I
titanium tetrachloride, which is subsequently purified and converted to
3 ?' W0 b: H+ p5 y& vtitanium dioxide either by direct thermal oxidation or by reaction with
" |& K$ \6 N) o" p; F! }! A0 @. d& F2 Psteam in the vapour phase. Alternatively, concentrated hydrochloric- ?9 v; q5 d9 x# f& ]. E
acid can be reacted with the titanium-containing mineral to form a
0 P% Y, d, E0 o8 V* Xsolution of titanium tetrachloride, which is then further purified and9 C# V7 ?, g/ i, S9 T9 O
converted to titanium dioxide by hydrolysis. The titanium dioxide is+ X1 o5 {# b# E, W6 w* H
filtered, washed, and calcined.. e9 J" O; S$ o( F3 l7 L
Commercial titanium dioxide may be coated with small amounts of X" d0 v) {) i* ]' t+ E5 r
alumina and/or silica to improve the technological properties of the0 u$ E/ ^/ V3 s: q4 O5 y+ q0 E
product.
. m9 j& v' E, hC.A.S. number 13463-67-7
- P9 C% M$ V! c* V* wChemical formula TiO2+ _ V, h! o! ?6 H& e! e# ~. c
Formula weight
2 B, b" c0 s2 y* `: ?" L9 i79.88
7 r' g; v" S8 N6 dAssay
$ h* u( |* ~% |# [Not less than 99.0% on the dried basis (on an aluminium oxide and" D2 T4 a) E5 l$ p1 p( Y. S% s* ^
silicon dioxide-free basis)
3 G/ \# u' N) D* O% M4 M" xDESCRIPTION
1 G1 N; M8 u! X) S! k- N% e9 Z8 K2 aWhite to slightly coloured powder
5 b4 n4 Q. w- wFUNCTIONAL USES7 r4 m# K1 j& D7 l/ O
Colour7 X/ D" C: ~- {# S2 L
CHARACTERISTICS7 G( D" V2 L6 g1 u9 R) ^( r3 b
IDENTIFICATION
: p7 V( H3 L( G4 Q7 Y9 N5 W+ }Solubility (Vol. 4): z3 ^5 c5 }& B5 ?6 R% t: C3 p' x
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic$ d& A0 G2 m, p: C/ o4 z; {
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated3 G9 \) v0 n" R
sulfuric acid.% i+ H9 s; G& c+ ~, N- j" u
Colour reaction
9 F" f% S/ b( _0 I4 v A- SAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
+ n0 T U. ]: B. }& isulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
7 G8 m% c: }3 q( P% pwater and filter. To 5 ml of this clear filtrate, add a few drops of: `8 z" P% a. w6 v9 _1 b
hydrogen peroxide; an orange-red colour appears immediately.
" C2 F% p! ~, x RPURITY5 ?6 }8 u7 C/ C0 y, j/ j
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
# t. S. \4 y, kLoss on ignition (Vol. 4)
4 i6 W2 b' B+ J/ {4 LNot more than 1.0% (800o) on the dried basis
9 ]) B7 a: k! wAluminium oxide and/or5 `5 c3 G* V: O3 L, R
silicon dioxide& V, V$ h- B. l, t0 n/ R$ Z3 J
Not more than 2%, either singly or combined. x6 ?: B0 i5 ?
See descriptions under TESTS
( G: m9 s* ~$ jAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing7 e$ X) A7 T; w. ]7 h2 ^
alumina or silica.: O2 s+ y0 X1 ?6 D- w& c/ A
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and+ |: s* `6 K) U0 G* H
place on a steam bath for 30 min with occasional stirring. Filter
0 N5 L& L! P. K3 g& p" x5 Othrough a Gooch crucible fitted with a glass fibre filter paper. Wash3 J* s3 w( i( l% O
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
D" H+ x9 E# o- ocombined filtrate and washings to dryness, and ignite at a dull red
8 ]1 C* p; f* F. c$ `heat to constant weight.
+ H% o0 b: R2 I$ ?0 x0 Q) ~* L9 mWater-soluble matter5 `+ _; S i' ]) F, F7 r S
(Vol. 4)
, E) m/ D1 h/ x/ dNot more than 0.5%+ Q, {" }( t, L+ h5 S( T
Proceed as directed under acid-soluble substances (above), using
; p0 P- o' V K7 gwater in place of 0.5 N hydrochloric acid.. P: R X! q5 y8 B# J
Impurities soluble in 0.5 N
8 \) k7 a5 q8 a& q; h) |" D* t4 Nhydrochloric acid
9 U7 Y" ~8 f4 h- ]Antimony Not more than 2 mg/kg
) z( Y7 F( B, l% j ZSee description under TESTS
/ h. l9 N% f: n6 H F9 tArsenic Not more than 1 mg/kg' @. k9 d5 K8 T9 m
See description under TESTS4 U! x3 y( O7 G, Y' F Z# c
Cadmium Not more than 1 mg/kg2 ^ Q7 B! S# z9 v0 R9 e4 r
See description under TESTS4 }" ~: f' @# H1 T) t _' \0 N
Lead2 D B/ K: k6 s8 p4 V
Not more than 10 mg/kg
: \* L) @: s/ R- KSee description under TESTS# w+ g+ k( p5 N6 {, M7 @3 T( }9 ~
Mercury (Vol. 4) Not more than 1 mg/kg
4 c# M/ ^7 W9 f$ }& X4 M; B/ @Determine using the cold vapour atomic absorption technique. Select a' p% ]6 i8 Y0 r3 m+ f* H; [
sample size appropriate to the specified level
y" f( N8 `% g% iTESTS6 f- L/ A) g3 c- \8 m6 A* H
PURITY TESTS
2 o) t- ~2 T& oImpurities soluble in 0.5 N
) z$ f5 a) Y* S6 _2 l0 Mhydrochloric acid
2 G7 \8 Z; ]8 yAntimony, arsenic,2 f, n! g4 |( T1 \2 Y9 x5 y
cadmium and lead
' M( y! b' J) \(Vol.4)% e& k2 D: `, q1 J
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
2 H" f( i% }- H) yhydrochloric acid, cover with a watch glass, and heat to boiling on a+ b4 p0 A, L0 A8 R7 {- x( G( a( L
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
; h& O) p: c% P/ G' L" |% Ycentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved2 r' P2 B- F$ A$ R" \/ J
material settles. Decant the supernatant extract through a Whatman6 n( \3 ]! f# r$ k0 K; z6 L9 s) \7 u
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
. G" ^0 c$ N+ R4 S; hvolumetric flask and retaining as much as possible of the undissolved; N7 E0 t- P- N
material in the centrifuge bottle. Add 10 ml of hot water to the original% c2 Z s' z: m; Y; R
beaker, washing off the watch glass with the water, and pour the9 I' A4 j' `: _9 i) N
contents into the centrifuge bottle. Form a slurry, using a glass stirring
1 L5 V- h& D: Irod, and centrifuge. Decant through the same filter paper, and collect' m( y$ ]. \6 l) [2 t
the washings in the volumetric flask containing the initial extract.
' ]' B" F$ }0 `, m4 w. g7 J, BRepeat the entire washing process two more times. Finally, wash the6 l* x% j% `% F9 Y+ D
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask/ f1 \$ r1 V8 U) g% }
to room temperature, dilute to volume with water, and mix.8 q- }" }" m- k: j6 e
Determine antimony, cadmium, and lead using an AAS/ICP-AES
^8 y8 N/ c. Ltechnique appropriate to the specified level. Determine arsenic using the
0 g* |: N8 P; G1 h) F' JICP-AES/AAS-hydride technique. Alternatively, determine arsenic using6 r3 I6 Z$ t" W' ?0 c0 R
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
& t; F! x X& j+ T& y+ }1 g. The selection of sample size and method of sample preparation( T; ~) _& b9 `6 _6 a' H* J
may be based on the principles of the methods described in Volume 4.4 K0 X4 X2 i6 z5 I
Aluminium oxide Reagents and sample solutions
( s8 d3 _) w" h& C0 x+ K0.01 N Zinc Sulfate2 A6 w2 o9 T: W: K/ i% u/ J# L
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
) }* o4 o* w! u8 wmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg3 p5 z7 o: m$ }
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
) m4 D' V7 C% F! C) Z" qconcentrated hydrochloric acid, heating gently to effect solution, then
P. N/ @- }2 E6 ?" ]2 itransfer the solution into a 1000-ml volumetric flask, dilute to volume
/ ]( ]. R* I1 s/ `0 G! awith water, and mix. Transfer a 10 ml aliquot of this solution into a 500' a( i1 B- Y* I( B( |! U
ml Erlenmeyer flask containing 90 ml of water and 3 ml of% R3 V& @. c3 R7 X. f
concentrated hydrochloric acid, add 1 drop of methyl orange TS and" U5 S) |$ M4 A, T
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
; d9 X$ M! t8 [7 Jdropwise, ammonia solution (1 in 5) until the colour is just completely S) w& S+ b; O0 w
changed from red to orange-yellow. Then, add:7 g( F$ O; l9 F# O" `4 v$ x0 @! ~; [! J4 a
(a): 10 ml of ammonium acetate buffer solution (77 g of" N/ @' f7 Z( q# p/ B9 M
ammonium acetate plus 10 ml of glacial acetic acid, dilute to' h3 Y( J) D0 o) a/ Z3 {$ k9 f2 n* {
1000 ml with water) and
, ]3 d2 E* N) \& z7 P(b): 10 ml of diammonium hydrogen phosphate solution (150 g1 L% D5 D: j; T6 f f( t* D
of diammonium hydrogen phosphate in 700 ml of water,
) K8 t4 v4 M6 w. aadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
U# G* @4 X Mthen dilute to 1000 ml with water).
/ C8 n' I" [7 k7 l3 ]/ E) E' f9 HBoil the solution for 5 min, cool it quickly to room temperature in a) [2 G: S: V0 A% I
stream of running water, add 3 drops of xylenol orange TS, and mix.- c1 J# x( o4 X/ c; W/ O# h; p1 p
Using the zinc sulfate solution as titrant, titrate the solution to the first* O1 Q- `. g* G) i& t5 f$ u
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
8 x9 N, j1 M* g8 ]0 PThis titration should be performed quickly near the end-point by
. r9 r! O, A" o3 k! Aadding rapidly 0.2 ml increments of the titrant until the first colour
8 l0 \( ]' s. L; _6 k# i% tchange occurs; although the colour will fade in 5-10 sec, it is the true' n( S1 O, |6 F* B5 f& i" [
end-point. Failure to observe the first colour change will result in an
( p2 w% n7 Y3 F* Q0 X& M+ a2 V uincorrect titration. The fading end-point does not occur at the second
9 [3 `& Y, Z: h+ i+ ^7 D) |3 yend-point.)
5 Z3 P1 y6 O. k9 h( M' NAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a; ?0 ~* K; p2 H2 l% ^1 a: _
stream of running water. Titrate this solution, using the zinc sulfate
; ~+ V$ y: D0 h7 b! h5 `solution as titrant, to the same fugitive yellow-brown or pink end-point" N6 y5 o% @% T h" @7 J
as described above.( [; X' Z w& ?* L4 u4 p1 B
Calculate the titre T of zinc sulfate solution by the formula:+ ]. E6 R1 H# @( W1 k# f9 v
T = 18.896 W / V/ T3 U# j$ A- @( L
where; B7 \0 u9 e6 [8 n( c$ B/ y
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution9 p9 r& o* _% Z, b, I Q
W is the mass (g) of aluminium wire" d2 ]5 Z9 r! F
V is the ml of the zinc sulfate solution consumed in the
+ J# S: k& g% L, c4 J" g# G' n% @second titration
9 W$ F# Y/ P1 z$ |0 C18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and5 z8 z) x1 b8 M4 M3 b
R is the ratio of the formula weight of aluminium oxide to5 {' t" M! B5 {$ Q) \
that of elemental aluminium.' P6 r' U: {6 D; P# F! C8 i
Sample Solution A- H c3 k1 _9 i2 i& X
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica- f3 d6 T. ]* A5 h: u8 f
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).. u' u2 C+ h- v4 ?0 M8 P
(Note: Do not use more sodium bisulfate than specified, as an excess
# r; ]: Y6 v4 Econcentration of salt will interfere with the EDTA titration later on in the# ]; l* r0 H4 i/ Y9 N
procedure.) Begin heating the flask at low heat on a hot plate, and
, s" {5 W0 l+ s, fthen gradually raise the temperature until full heat is reached.
2 e$ v3 G/ h0 o5 `(Caution: perform this procedure in a well ventilated area. ) When
0 b, r0 J. P+ H8 Cspattering has stopped and light fumes of SO3 appear, heat in the full
! I$ \; E) E8 m" p( `7 Aflame of a Meeker burner, with the flask tilted so that the fusion of the
& T* l1 Q2 l9 }/ n( |7 [# @sample and sodium bisulfate is concentrated at one end of the flask.& {7 \, {0 x6 f% u' c) R( T
Swirl constantly until the melt is clear (except for silica content), but' I- j8 [) d# L' E9 J d0 s6 F
guard against prolonged heating to avoid precipitation of titanium$ S0 Y( t& {; S% D
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until! ?: s1 F/ i6 `( c: ~1 z5 H- G
the mass has dissolved and a clear solution results. Cool, and dilute to
8 [: [6 i3 _$ v3 a120 ml with water. Introduce a magnetic stir bar into the flask./ ? S3 q' ^9 j/ [9 I- _
Sample Solution B
' @; p. I( L/ S. H5 QPrepare 200 ml of an approximately 6.25 M solution of sodium
+ X; O" N% B9 n! V# G- {) }hydroxide. Add 65 ml of this solution to Sample Solution A, while( p. p+ w6 E0 o/ _
stirring with the magnetic stirrer; pour the remaining 135 ml of the* a0 M0 E5 \, d) H- U/ r. N: Z
alkali solution into a 500-ml volumetric flask.
8 x0 J: H3 T1 m& ?1 a( U- o" xSlowly, with constant stirring, add the sample mixture to the alkali
# X/ ^1 Y5 h M$ g& U" l6 Rsolution in the 500-ml volumetric flask; dilute to volume with water,! |5 d3 I4 ~+ u% x+ C
and mix. (Note: If the procedure is delayed at this point for more than
5 O- x/ ?2 _+ P' Y2 hours, store the contents of the volumetric flask in a polyethylene
( t8 V! l5 z+ jbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),: K7 S) H3 g- _9 p, o L
then filter the supernatant liquid through a very fine filter paper. Label3 S* x* I6 ^2 Q0 W( s0 A+ N/ W
the filtrate Sample Solution B.# I) z& m7 i: |
Sample Solution C
1 d% Z7 G! h* P* k" W, M" l$ _Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer" c/ O( E6 y+ I
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid1 `' y- ~8 c9 I, [9 t+ u$ C9 n# P
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02+ p2 K: ?% d% P6 L
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
* i+ c9 P8 Q B6 N0 Tknown, calculate the optimum volume of EDTA solution to be added
" L( ~ U: L; y' T( `) ?. W# Vby the formula: (4 x % Al2O3) + 5.]
! @( h, X* Z9 g& M" @Add, dropwise, ammonia solution (1 in 5) until the colour is just* }- h! W5 B- U4 u
completely changed from red to orange-yellow. Then add10 ml each& m# C& n) h1 b9 e$ E, H
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to8 A/ {4 ~! A; b% |# a
room temperature in a stream of running water, add 3 drops of xylenol4 S! d2 H I# f/ J% X
orange TS, and mix. If the solution is purple, yellow-brown, or pink,7 Y0 } Z' c3 y& \ c2 a* b
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
, f2 U/ n/ j) \pH, a pink colour indicates that not enough of the EDTA solution has
, m7 F. A9 H4 i5 `7 J: A X2 Q- fbeen added, in which case, discard the solution and repeat this
; q% O. K3 l9 [ U+ X2 E+ h$ D! vprocedure with another 100 ml of Sample Solution B, using 50 ml,
. G. i$ C# l0 L4 h$ F! Z8 Erather than 25 ml, of 0.02 M disodium EDTA.. l7 F# H8 t; y" I x" Q) Q6 A
Procedure/ D0 X7 V! {6 a
Using the standardized zinc sulfate solution as titrant, titrate Sample* H& _; M& E/ S s1 r4 Z( ^$ d
Solution C to the first yellow-brown or pink end-point that persists for) r, p. ^* J$ t
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first7 T& _7 `8 {6 D1 f& J. J
titration should require more than 8 ml of titrant, but for more accurate
3 V. W! y( o* D+ p4 ^ x1 N+ q Pwork a titration of 10-15 ml is desirable.9 {. ]2 R7 ~4 C% O0 R5 N
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
+ w7 y5 k/ F# mmin, and cool in a stream of running water. Titrate this solution, using/ S: p3 ^0 W% n( U/ X+ ?' F7 n* Z
the standardized zinc sulfate solution as titrant, to the same fugitive k7 h/ C5 Y0 B% `
yellow-brown or pink end-point as described above.
0 b$ m7 C. |* XCalculation:1 n% c- |7 _+ D
Calculate the percentage of aluminium oxide (Al2O3) in the sample
. R$ T& @+ i' D* q% L! y! Vtaken by the formula:
8 T) h. q0 j6 C+ w3 T( D% Al2O3 = 100 × (0.005VT)/S
0 C# f" Z8 V. C, z3 d D% bwhere9 J7 i$ j' n/ Z) d
V is the number of ml of 0.01 N zinc sulfate consumed in
8 |+ v# R7 b" l) C( `; Z$ {, athe second titration,. h1 v7 ^% [' |$ E1 X
T is the titre of the zinc sulfate solution,
5 T+ H7 D2 q& @S is the mass (g) of the sample taken, and3 Q# l1 m( a |- D$ X) Y
0.005 = 500 ml / (1000mg/g × 100 ml).
- z" p* k: a: m( R+ }1 T$ dSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica9 F5 |- [) I/ n" Q0 R/ h6 e8 u" ]9 d) E
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).8 Q- ^- j+ H, C4 Y6 c* f% z ?' [( Y8 P
Heat gently over a Meeker burner, while swirling the flask, until
1 G: F8 h- c& F5 A/ @decomposition and fusion are complete and the melt is clear, except
0 s6 l# t2 e+ Y5 Ufor the silica content, and then cool. (Caution: Do not overheat the
5 d1 z4 q9 u8 L# H! l! rcontents of the flask at the beginning, and heat cautiously during' L+ q0 u# w0 R. B" v/ p* T
fusion to avoid spattering.)' [9 U7 A- L, {1 g9 K& j
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
; ?- N4 I) f" z# J; q6 s `/ p4 Ocarefully and slowly until the melt is dissolved. Cool, and carefully add
$ k& ?' v1 ~$ k: W( V150 ml of water by pouring very small portions down the sides of the
t4 ~) x4 `/ H, w* U: uflask, with frequent swirling to avoid over-heating and spattering. Allow4 {2 Q1 n8 G; @- I I R9 K1 g
the contents of the flask to cool, and filter through fine ashless filter! j/ `7 o3 d3 \. n. z% i- C* Z5 R: z Q
paper, using a 60 degree gravity funnel. Rinse out all the silica from6 T0 ~7 M2 |/ V2 f
the flask onto the filter paper with sulfuric acid solution (1 in 10).' f6 S; v5 {" I, b3 H. o
Transfer the filter paper and its contents into a platinum crucible, dry in
9 L: Z* D3 W; z, \3 j* E; w/ ean oven at 1200, and heat the partly covered crucible over a Bunsen* ]/ m5 q( G9 R" l& ?3 b
burner. To prevent flaming of the filter paper, first heat the cover from: w( K% ^+ `% r& \! Z) g x
above, and then the crucible from below.$ f/ C2 ]+ _) E' `7 ~
When the filter paper is consumed, transfer the crucible to a muffle
9 }7 O- [' m- U- O+ m2 ifurnace and ignite at 1000o for 30 min. Cool in a desiccator, and0 Y1 \$ K6 H: T/ i
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
' v5 n+ h, F4 Q: thydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first( j p0 ?# N/ u, l) u) k
on a low-heat hot plate (to remove the HF) and then over a Bunsen
: ~$ J" j/ t2 A% o+ bburner (to remove the H2SO4). Take precautions to avoid spattering,1 _; a1 g2 t1 h1 o
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
3 Y {' j7 p* L6 wdesiccator, and weigh again. Record the difference between the two6 g& U- j/ N- v
weights as the content of SiO2 in the sample.
4 l3 Z3 A! {8 E& ^5 a l; M, PMETHOD OF ASSAY
8 b, a9 r2 a' I& L" GAccurately weigh about 150 mg of the sample, previously dried at 105o
2 u4 `* ?! ~+ x0 Z' g. {3 t) N, M9 pfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
% k- z5 j& H3 Z8 P: I$ band shake until a homogeneous, milky suspension is obtained. Add 303 w- H9 K" [& r5 l- K
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
: B& U, S0 [" M. D' u$ K* Vheat gently, then heat strongly until a clear solution is obtained. Cool,& Q h9 ^' T7 p. |1 L5 o& z7 I
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
0 Z; _$ k0 k# ~+ Q2 xacid, and stir. Add 3 g of aluminium metal, and immediately insert a' j) q, E& G: Q$ r% C7 @
rubber stopper fitted with a U-shaped glass tube while immersing the7 A' u R2 ?! b
other end of the U-tube into a saturated solution of sodium. o6 F2 s6 n8 I+ r" e
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
. e+ n8 Q+ {9 s2 T% m$ Uhydrogen. Allow to stand for a few minutes after the aluminium metal! y* r: {6 G2 _- r% k
has dissolved completely to produce a transparent purple solution.4 K+ E) H( _5 n6 N3 g% s& l- l
Cool to below 50o in running water, and remove the rubber stopper
, W, ^: Y7 h5 `carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate/ V$ u% E5 k+ z9 ^% A
solution as an indicator, and immediately titrate with 0.2 N ferric$ X; u8 P/ K) g. q$ L* ?
ammonium sulfate until a faint brown colour that persists for 30
3 }* U' C: {. l' D1 V" ]. m4 Dseconds is obtained. Perform a blank determination and make any- I9 X/ `( \% J( }: A/ P3 o
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
# c9 w9 _( h' s6 L0 cequivalent to 7.990 mg of TiO2.
6 {$ `5 V5 ?, c: E( z; {* | |
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