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二氧化钛(钛白粉)
二氧化钛(钛白粉)$ V2 I) E' d2 F) h
7 D- e4 }- O. E* f5 {# p6 X- u, y
JECFA关于二氧化钛(钛白粉)的结论: k, {' _* D2 T& c
: |" k/ g) S# f* ?: J; H摘要: 2006年JECFA关于二氧化钛的结论2 Q* v; `) Q9 g9 D( {3 c
ADI值:不作限制。
- i, C6 p& ?- i- C8 O7 [功能:着色剂. n! R* u) Z) {( p0 I# p! e. ~4 `
% h- C8 X1 T9 o6 b7 r1 H$ ~, T" K
TITANIUM DIOXIDE! ]- C4 J4 o! a# q8 t# a
Prepared at the 67th JECFA (2006) and published in FAO JECFA) G0 t" M J$ z. J0 X8 X9 I
Monographs 3 (2006), superseding specifications prepared at the 63rd: ], Z' T0 P/ u9 d, X
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
4 z6 N ]+ @& ?' p2 @ o. hCombined Compendium of Food Additive Specifications, FAO JECFA
& P% l6 Q5 a5 T3 k& e+ }- `3 H' YMonographs 1 (2005). An ADI “not limited” was established at the 13th
& A. O1 B0 V! gJECFA (1969).
6 C$ |# a1 H% e+ }1 f D9 X! ASYNONYMS
) r! R& D8 x! G) n! CTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
' a8 N% N) j7 tDEFINITION0 M. h+ T g9 l1 e9 f
Titanium dioxide is produced by either the sulfate or the chloride
N8 N4 N+ e; W. f2 Z5 tprocess. Processing conditions determine the form (anatase or rutile' N/ Y+ a8 `% m, F
structure) of the final product.9 a- s& E7 A- v* z4 G+ U
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)* M; S0 Y; g3 q4 ]2 J' T; Z# \
or ilmenite and titanium slag. After a series of purification steps, the# {! a+ G, f1 j0 F2 y, O% e7 M) V, a
isolated titanium dioxide is finally washed with water, calcined, and
0 B8 j/ f) L( U W! m. ^micronized.
* E* A5 H5 Q* i* u, v+ P. F( O6 G% QIn the chloride process, chlorine gas is reacted with a titaniumcontaining
) O. {+ n! ?& @& q3 Emineral under reducing conditions to form anhydrous
, Q: U; i+ O( B0 [: b) B: C. `* Stitanium tetrachloride, which is subsequently purified and converted to. B) |1 Z: U" w' ^+ g
titanium dioxide either by direct thermal oxidation or by reaction with
6 H- o2 d P/ Qsteam in the vapour phase. Alternatively, concentrated hydrochloric
" i5 e* s6 ^" e$ \; [5 lacid can be reacted with the titanium-containing mineral to form a5 \/ X3 F6 D& h3 E
solution of titanium tetrachloride, which is then further purified and5 P8 Y' A0 Q7 g# Q& k+ ~9 Q' H
converted to titanium dioxide by hydrolysis. The titanium dioxide is E3 Z; ^4 a E5 B* K9 ^. Q) y& Q
filtered, washed, and calcined.
% R8 P0 G* y0 R0 {: r& ]: Z7 Y2 OCommercial titanium dioxide may be coated with small amounts of
8 Z6 _% n! s6 {) x% zalumina and/or silica to improve the technological properties of the
3 h* j" B8 Z& R6 J3 s3 O; Rproduct.
! J/ \0 h0 w* H0 ]' y" W( zC.A.S. number 13463-67-77 ^6 {+ N* g- w& n# U
Chemical formula TiO2- q3 f) d* D2 [. @4 `% Z
Formula weight! L, S0 E3 w) a1 d8 W* d, j
79.88
4 K& h4 V; M* E& Z5 M0 rAssay* S( i4 n$ }( i( w/ j0 o) X
Not less than 99.0% on the dried basis (on an aluminium oxide and
! l1 y% J* |" I3 m# @4 t# {. ^( `0 tsilicon dioxide-free basis)
6 T8 v p6 R! j* Z+ [. wDESCRIPTION
- C- L8 ]! n) J6 j9 O5 h, YWhite to slightly coloured powder
8 U$ \& c; d3 U; o$ UFUNCTIONAL USES1 Z9 h1 W* A5 W4 z! g4 J+ T/ v
Colour
5 m1 b* E& w; c! s" U7 ]3 LCHARACTERISTICS
* k7 ` B& b4 n' OIDENTIFICATION7 @$ I/ S+ {( F
Solubility (Vol. 4)
. [; Z; v$ ?* H% jInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
. j% j* s8 V6 t0 _( O5 C9 tsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
. M, L* y8 O% V6 X1 Lsulfuric acid.
& b" q" n/ |# J6 _, }: u1 o6 XColour reaction
. A/ G G3 \; `0 v1 x' mAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of1 U9 X1 E5 ^& D9 u# _+ l
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
# W, o9 e7 L ]4 _. zwater and filter. To 5 ml of this clear filtrate, add a few drops of" e1 P1 D& w0 F4 }' W
hydrogen peroxide; an orange-red colour appears immediately.
; {2 U5 t; l7 Q" x* A2 P. ~( sPURITY: L# e$ m6 W5 i6 W' ]
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h) H' t. o" ~: a. ?$ W) I! ?
Loss on ignition (Vol. 4)
4 g$ |0 o, o* u. b' Z9 ANot more than 1.0% (800o) on the dried basis
+ o8 f! N. B+ y7 H2 v2 J- B" AAluminium oxide and/or
0 i* p) y1 D0 M' asilicon dioxide
* d. m. b# K7 i8 W7 f' ^Not more than 2%, either singly or combined
2 t0 P, j+ |" ~. F4 `. Q0 ]4 OSee descriptions under TESTS/ ]+ u! G/ e, j& |3 l: C
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
: E0 j0 \9 q+ x7 M8 U4 {7 `alumina or silica.. u6 \' S0 W$ ] M5 L* v0 Y
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
3 p& O7 r# w, M+ r7 f6 u) W$ lplace on a steam bath for 30 min with occasional stirring. Filter
+ D4 `, h: k q3 cthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
5 s; g. V* Y. _! E% Jwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the6 H7 i( \- B6 X' T
combined filtrate and washings to dryness, and ignite at a dull red
: j: z2 p' F& Eheat to constant weight.
5 E, C1 X0 B' f7 dWater-soluble matter7 k6 ^$ M8 e& i
(Vol. 4)' r1 n; |2 r9 C+ W, U) h2 Y4 [
Not more than 0.5%" ?; D# W- ~. w7 E. D6 l2 i8 g
Proceed as directed under acid-soluble substances (above), using/ x* p& q7 P0 }# _
water in place of 0.5 N hydrochloric acid.
9 Y; N8 O! |9 H% [- NImpurities soluble in 0.5 N
2 P% V% m( i! B9 Ihydrochloric acid5 y* B- A7 C. O% S, u! W
Antimony Not more than 2 mg/kg) y; c0 ~' k' m- ]7 `8 F
See description under TESTS
; \6 y: k3 \7 f1 d7 \1 e% rArsenic Not more than 1 mg/kg
% v7 i7 A4 A, C( r7 F. C. eSee description under TESTS6 z: H$ X0 h7 e# M- P. g; _
Cadmium Not more than 1 mg/kg8 `" u; x7 k. y9 v4 Q* Z
See description under TESTS
: N$ a; {& M) kLead @, v1 c1 ^9 h/ b
Not more than 10 mg/kg
& u% R" _% t( C2 Z5 OSee description under TESTS9 C0 l6 U# x5 V1 c4 p
Mercury (Vol. 4) Not more than 1 mg/kg# s K. Z9 X5 z$ P: N
Determine using the cold vapour atomic absorption technique. Select a) [1 }& ^# \ B, M$ G5 C
sample size appropriate to the specified level: o6 C4 A8 z* K) G
TESTS& g, X: g) W0 ]/ t# K0 P
PURITY TESTS6 w% l+ f! y# X2 b
Impurities soluble in 0.5 N/ t- R$ o! r9 D0 j8 j9 K* j2 a
hydrochloric acid4 x/ g! @/ T6 J. Z, B- Y
Antimony, arsenic,! p$ X% Y8 S2 S( S7 H
cadmium and lead
# e- r0 m. [( F M, r' h3 i(Vol.4)3 K8 J$ M/ a! K" B* h9 x
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
3 B0 ~0 Y4 | `8 Y3 Q0 t5 [1 F9 hhydrochloric acid, cover with a watch glass, and heat to boiling on a
% a2 T4 J+ T9 i5 Hhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
# N- F8 C% W4 ?) Z# b9 H. }centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved1 y* N& r5 \. j( L7 f
material settles. Decant the supernatant extract through a Whatman
. U. ~3 D2 W, L# {1 f/ M0 fNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
1 [; b$ W, E Cvolumetric flask and retaining as much as possible of the undissolved
. M4 A; f8 I) W/ v% zmaterial in the centrifuge bottle. Add 10 ml of hot water to the original. U5 X2 M4 M2 U! q+ P
beaker, washing off the watch glass with the water, and pour the
$ k3 Q- n. k$ V$ Rcontents into the centrifuge bottle. Form a slurry, using a glass stirring+ e, i) N7 o; E
rod, and centrifuge. Decant through the same filter paper, and collect/ O& v" q2 ]; ^
the washings in the volumetric flask containing the initial extract.
. t, ]5 O/ \, K" L6 v" \: ZRepeat the entire washing process two more times. Finally, wash the( K7 L9 w; U" ]) X% J$ r
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask9 G3 A* ?) u O5 ^, z6 g4 I, |9 J3 s; n8 d
to room temperature, dilute to volume with water, and mix.$ [4 N1 Q% G" T: ]& ~
Determine antimony, cadmium, and lead using an AAS/ICP-AES; \+ g! d1 H- N v7 S; g( ~0 s
technique appropriate to the specified level. Determine arsenic using the
7 D: O+ P) g" GICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
" }2 S0 i4 E$ M5 S3 M' ^Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
1 Y0 m* j% r- p ]! \& ]! l1 J1 g. The selection of sample size and method of sample preparation
, ?2 U9 H3 J' \; r5 X. L& A& Q4 J4 Vmay be based on the principles of the methods described in Volume 4.3 ?6 T$ e9 `8 _% c% M: X
Aluminium oxide Reagents and sample solutions+ h0 B0 k( q8 J+ ~
0.01 N Zinc Sulfate5 X7 p/ H% W5 X, d
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to$ ^4 p2 c1 @9 n0 A& w6 e* k/ ]
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
; ^- d4 M1 A0 J& S( O. H8 Dof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
: |6 X) j, ]3 A+ U# q. Pconcentrated hydrochloric acid, heating gently to effect solution, then
2 s" G. b, ]( l; ]6 @, Wtransfer the solution into a 1000-ml volumetric flask, dilute to volume
& r9 Z4 _9 m) U1 \+ S Pwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
/ a# m5 S7 a0 xml Erlenmeyer flask containing 90 ml of water and 3 ml of0 R" L( C" D2 t" ^/ o6 o/ R4 C
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
6 B& B) H- o* b25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
- R' j( ?! @4 l% _6 q/ Q% fdropwise, ammonia solution (1 in 5) until the colour is just completely
6 v0 D' o4 o* b( r+ B2 T7 g) vchanged from red to orange-yellow. Then, add:9 {7 Q7 _1 s* y4 c
(a): 10 ml of ammonium acetate buffer solution (77 g of
2 Q9 S. q: U0 g m6 O/ oammonium acetate plus 10 ml of glacial acetic acid, dilute to
2 f; R9 _; ~/ l4 ~8 T9 d; K1000 ml with water) and: c( w' l) k1 U/ H6 M9 r# ^* B6 S
(b): 10 ml of diammonium hydrogen phosphate solution (150 g: G9 E5 d3 I3 h5 L& Q2 W# y
of diammonium hydrogen phosphate in 700 ml of water,+ J; w" V5 F/ g2 ?7 N
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
8 u/ v% Z" C y; x8 a* \1 uthen dilute to 1000 ml with water).
& \9 u) f3 _4 `9 {' b/ eBoil the solution for 5 min, cool it quickly to room temperature in a6 J; H1 P$ u5 o
stream of running water, add 3 drops of xylenol orange TS, and mix.
. N2 {; A4 g5 c: _+ V/ ]! lUsing the zinc sulfate solution as titrant, titrate the solution to the first
2 d7 @* x$ Y) ~6 z6 J6 g4 ~% eyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
w$ |( k) r( }# aThis titration should be performed quickly near the end-point by
! B( r5 U9 s4 L3 t0 gadding rapidly 0.2 ml increments of the titrant until the first colour
& L- j$ [0 }/ C0 pchange occurs; although the colour will fade in 5-10 sec, it is the true" e0 g3 k3 e+ |5 `& S
end-point. Failure to observe the first colour change will result in an
3 v2 w2 C% U: O9 L& bincorrect titration. The fading end-point does not occur at the second5 @" i2 q! b& n9 o, _) L) a
end-point.)% J7 G/ C( T& f# R. x- }
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a+ O& w! q) A; P" h! r
stream of running water. Titrate this solution, using the zinc sulfate
+ Z8 D" g* L4 R" U" Psolution as titrant, to the same fugitive yellow-brown or pink end-point
, ~( S3 O2 c9 n+ R( h8 a0 bas described above.
; K+ E% }! t2 h( MCalculate the titre T of zinc sulfate solution by the formula:# _; @9 O: C; N0 Z1 q
T = 18.896 W / V
' Q: n$ K9 |; ~' l+ Bwhere% v: B. e# c/ c, \+ {) h* n* y, x
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
) f7 K- g0 T; UW is the mass (g) of aluminium wire
8 H. ~: D& i: O L" V, t' CV is the ml of the zinc sulfate solution consumed in the
, Z1 C: A% ^7 ?7 \second titration; q4 b& D1 c1 D; O+ b
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
+ e3 m, U- v# s+ k3 w* p) ~R is the ratio of the formula weight of aluminium oxide to0 L( k) y: R9 D7 m6 M, F. C
that of elemental aluminium.* q. N- t8 U. Z( |' k* M
Sample Solution A
: @- @/ B5 z8 n( H& wAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica1 ~/ p& a B, T/ F1 w
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O)., |5 i8 \, g$ J" Y- C
(Note: Do not use more sodium bisulfate than specified, as an excess
) d/ N( O4 F& g5 Q# W( E6 _concentration of salt will interfere with the EDTA titration later on in the# A. Y9 n: ] f5 U& c
procedure.) Begin heating the flask at low heat on a hot plate, and* \! `& Y) ]! V7 _5 w% j( R
then gradually raise the temperature until full heat is reached.
# R: ~" F" {& Q' |+ P C8 f: v(Caution: perform this procedure in a well ventilated area. ) When
6 f7 }0 q; H( t4 r0 Espattering has stopped and light fumes of SO3 appear, heat in the full/ t$ v0 F' {) p- Y
flame of a Meeker burner, with the flask tilted so that the fusion of the
* C& z0 @: r; Y3 zsample and sodium bisulfate is concentrated at one end of the flask.+ l. M2 |' H3 H0 y8 U; S6 P
Swirl constantly until the melt is clear (except for silica content), but
! f$ ^0 x6 n: M0 C- |guard against prolonged heating to avoid precipitation of titanium
2 l2 o5 x, O( v/ ]. ?dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
$ S7 \) D% U1 a/ \4 T: Lthe mass has dissolved and a clear solution results. Cool, and dilute to
8 l. ~4 k8 N& |- A a120 ml with water. Introduce a magnetic stir bar into the flask.* |2 u4 E9 Q. O
Sample Solution B
; S0 L& p+ E+ C6 l3 r! DPrepare 200 ml of an approximately 6.25 M solution of sodium: r; l9 Y$ V/ B* u+ L( U
hydroxide. Add 65 ml of this solution to Sample Solution A, while) J+ C9 n' B8 B) A
stirring with the magnetic stirrer; pour the remaining 135 ml of the
0 j; g1 v2 z! E" J5 r8 ralkali solution into a 500-ml volumetric flask.
. Q. @- H# `3 K" h2 qSlowly, with constant stirring, add the sample mixture to the alkali- n- i, T6 n$ _3 j
solution in the 500-ml volumetric flask; dilute to volume with water,- m8 k9 z. ?1 @
and mix. (Note: If the procedure is delayed at this point for more than- Q) q% O* n. `1 K+ _, Y" M4 s
2 hours, store the contents of the volumetric flask in a polyethylene
+ t8 E3 R! i7 t( @bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),, ~% B6 ^7 s J( P+ h! m
then filter the supernatant liquid through a very fine filter paper. Label7 [% S0 A& a% J/ j; j& l
the filtrate Sample Solution B.: O" `7 S2 X. S
Sample Solution C3 C9 u" n, r. A7 o5 P
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer2 Y" Q3 E/ e$ @8 @3 L
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid* ~/ a1 s: E& y0 ?3 R
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
; ]! i( b! r- c* _! W& G D( L }& H' L$ nM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is- w* }3 }" V& e7 j
known, calculate the optimum volume of EDTA solution to be added/ M& h* G9 v2 ^' A1 \/ g
by the formula: (4 x % Al2O3) + 5.]+ f- b I/ f7 G* L3 ]6 Z
Add, dropwise, ammonia solution (1 in 5) until the colour is just6 x" e4 F* k( s8 L, c1 |% w
completely changed from red to orange-yellow. Then add10 ml each6 j9 F8 @/ W" ?# R4 e
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
( }+ Y! {4 e7 Z: {5 ]5 c# Jroom temperature in a stream of running water, add 3 drops of xylenol
- k. ^8 @0 F4 f$ y$ W" j' Horange TS, and mix. If the solution is purple, yellow-brown, or pink,
3 M: q! C5 I2 w2 cbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
- j8 f$ e* \- Q2 y, ypH, a pink colour indicates that not enough of the EDTA solution has& o, O+ ]. ^+ I/ U$ Y
been added, in which case, discard the solution and repeat this
+ |' a: t& @# a8 s n8 Zprocedure with another 100 ml of Sample Solution B, using 50 ml,
/ W0 |4 I" M9 [5 Crather than 25 ml, of 0.02 M disodium EDTA.
- T2 i( y0 t3 V& i, u* n7 `Procedure# W |& R! i; ]
Using the standardized zinc sulfate solution as titrant, titrate Sample3 S2 I4 q, Y& A5 M. v3 z6 ~
Solution C to the first yellow-brown or pink end-point that persists for- b# U4 U& \ Q9 j4 ~* r( _" \) l
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first- ^+ \) u( r. f* p: M
titration should require more than 8 ml of titrant, but for more accurate
- t: `9 b; N& R# {/ M7 Xwork a titration of 10-15 ml is desirable.
: R: Y# _2 F3 ]3 k6 ~# KAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
5 W- y1 ?+ [3 T3 `+ x l6 O& D' cmin, and cool in a stream of running water. Titrate this solution, using7 k; E- _& L$ l% `# G# H3 E
the standardized zinc sulfate solution as titrant, to the same fugitive7 d" J+ B& ?' I% P
yellow-brown or pink end-point as described above.) V. }$ l$ m' n/ ?9 m* d
Calculation:. j) k) ~ q- ]- S
Calculate the percentage of aluminium oxide (Al2O3) in the sample
3 e! I' _6 a2 I) q/ V7 G# h% Gtaken by the formula:5 W; m( w' e4 Q! h
% Al2O3 = 100 × (0.005VT)/S
. s7 v/ K6 z* J6 `7 ^* q* Iwhere& K. u l2 @# K3 e. `: f+ Y9 z
V is the number of ml of 0.01 N zinc sulfate consumed in- v, X8 b% u8 R+ u
the second titration,
6 P) h$ B: p+ [: l2 K ZT is the titre of the zinc sulfate solution,$ X; V0 L" _% ~# O; g: M
S is the mass (g) of the sample taken, and
; d6 a; }, s. B0.005 = 500 ml / (1000mg/g × 100 ml).) ~9 M3 w; u& f( r3 J+ K
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica# _) p' p# w3 c, u* k
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).# d: F3 d! _: {8 E: q6 w j2 X, D! P
Heat gently over a Meeker burner, while swirling the flask, until5 L0 Q; R x% x: o
decomposition and fusion are complete and the melt is clear, except& {9 m5 b" ]$ S
for the silica content, and then cool. (Caution: Do not overheat the
# B! N& v; H; R, ~: v9 [contents of the flask at the beginning, and heat cautiously during
. h/ p# U7 N Z6 H; U; k7 e) Nfusion to avoid spattering.)
% N* t' S4 ~4 O. O. P9 oTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat) k1 d' X& G+ F( Z+ x! X
carefully and slowly until the melt is dissolved. Cool, and carefully add: a3 L9 u3 a+ ^5 Y# a
150 ml of water by pouring very small portions down the sides of the
9 Y1 E5 A+ `% N9 N+ ~+ D; dflask, with frequent swirling to avoid over-heating and spattering. Allow3 @ K* [7 F# Z& S j
the contents of the flask to cool, and filter through fine ashless filter! Z6 S1 E3 n+ J$ i/ C
paper, using a 60 degree gravity funnel. Rinse out all the silica from
# I0 h$ o' {0 A+ w, D6 p( Kthe flask onto the filter paper with sulfuric acid solution (1 in 10).& r, f8 x$ z7 u1 E! h+ c8 A
Transfer the filter paper and its contents into a platinum crucible, dry in+ A# T! C3 s7 r* f
an oven at 1200, and heat the partly covered crucible over a Bunsen7 G3 K, A4 P- P% P. `
burner. To prevent flaming of the filter paper, first heat the cover from% l4 a, D3 n6 ]# f" ?+ x
above, and then the crucible from below., E: D6 A& X# b
When the filter paper is consumed, transfer the crucible to a muffle
# T* d! Q9 _8 h( x5 Q& O% V6 Tfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
$ @# \, `5 f/ Y2 Oweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated6 p% p2 r9 A0 G, ~/ c5 D y
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first0 j7 Z! F A3 Z, A z
on a low-heat hot plate (to remove the HF) and then over a Bunsen
! A1 J$ [$ u5 e9 W: @burner (to remove the H2SO4). Take precautions to avoid spattering,7 u! o7 |2 t. d1 J* `0 V
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a7 m+ Y g0 ~/ Y2 x
desiccator, and weigh again. Record the difference between the two, X( y8 |' |3 j
weights as the content of SiO2 in the sample.
: F5 x' i# h, r1 R* ]8 KMETHOD OF ASSAY) o+ w" i2 a: K3 _0 Z
Accurately weigh about 150 mg of the sample, previously dried at 105o7 u; F, o& r4 q% n& J+ Q
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
) i1 j, K7 B' C4 \. |6 N1 U+ B- Pand shake until a homogeneous, milky suspension is obtained. Add 30
1 e3 d3 w+ t( y$ Nml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
- p+ k7 W" o" W4 W& zheat gently, then heat strongly until a clear solution is obtained. Cool,/ r0 e) d! c! x# J
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
! ]; B# D0 ]7 c( I6 Q7 y+ Vacid, and stir. Add 3 g of aluminium metal, and immediately insert a" n& m6 P( I$ ]& Q* S
rubber stopper fitted with a U-shaped glass tube while immersing the* ]% c; p$ S. o" A( C* i
other end of the U-tube into a saturated solution of sodium/ ] N, m" G' h% U. i( c5 a
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
# D5 n: }- o! _8 g3 V! K& Uhydrogen. Allow to stand for a few minutes after the aluminium metal$ }! p3 W s5 e) Q0 C4 Q
has dissolved completely to produce a transparent purple solution.* @8 W7 ^# P8 a
Cool to below 50o in running water, and remove the rubber stopper: r" l# _) s0 `/ ^9 ~
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
& \. {7 W8 ^) _( d# F1 `. ?( }% Ssolution as an indicator, and immediately titrate with 0.2 N ferric
& v" r, o5 n! L" h& |ammonium sulfate until a faint brown colour that persists for 306 n' S2 E& c E) c% K
seconds is obtained. Perform a blank determination and make any0 G+ C2 a+ T' D# i3 H9 `2 }
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
# C8 I( m q( x7 K5 D0 requivalent to 7.990 mg of TiO2.& F. g/ s3 Q& q; R/ p
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