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二氧化钛(钛白粉)
二氧化钛(钛白粉)
4 f% {$ a+ K$ O6 j5 ^. Y; Z- V. O f# t7 x/ U
JECFA关于二氧化钛(钛白粉)的结论1 w2 J; i% y H
& e0 m K9 G% [/ m摘要: 2006年JECFA关于二氧化钛的结论
" {- M- M6 F" E: ], B; ^: KADI值:不作限制。
. y. L* ?7 X% {/ `, r! W8 v功能:着色剂
, k5 d w9 |2 ^6 H" e' n+ }, ]8 l, E, D6 v% C
TITANIUM DIOXIDE
7 }5 F3 R4 }5 XPrepared at the 67th JECFA (2006) and published in FAO JECFA5 i: O7 A2 i: r7 w/ Y) k6 j% x
Monographs 3 (2006), superseding specifications prepared at the 63rd
: N. A; J8 Z; n, T' h) ^JECFA (2004) and published in FNP 52 Add 12 (2004) and in the; d% ~! `. @' _) [+ _! O6 V, Y9 I
Combined Compendium of Food Additive Specifications, FAO JECFA+ ?% T: o& Q% [7 [
Monographs 1 (2005). An ADI “not limited” was established at the 13th
& X6 @; A& D* [JECFA (1969).
+ ?+ Z% \. I% `" R9 RSYNONYMS
, r) ?- k2 e- [# L& T* t8 I6 dTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1713 U. b) b" A! V1 Y- n
DEFINITION6 o& R4 q* I0 X, i
Titanium dioxide is produced by either the sulfate or the chloride4 K( l9 k* t4 S" K2 g' V/ E9 x- D6 C
process. Processing conditions determine the form (anatase or rutile
/ h# {0 j$ ], zstructure) of the final product.5 e# e. C0 a6 c
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)9 v. T( r: V% u, N- ^+ u7 p) H
or ilmenite and titanium slag. After a series of purification steps, the/ y6 H/ o' r' U4 k+ _
isolated titanium dioxide is finally washed with water, calcined, and
+ A) {5 k* E( c/ v' Q8 kmicronized.
3 [! z. x" \0 V) F) V9 }. YIn the chloride process, chlorine gas is reacted with a titaniumcontaining
& p) c+ o* K" |' Omineral under reducing conditions to form anhydrous
# W! v& `1 U5 Q0 G7 {+ ctitanium tetrachloride, which is subsequently purified and converted to
9 z9 V5 ]) p0 i/ A _titanium dioxide either by direct thermal oxidation or by reaction with
5 p2 d+ K! Y: I. B$ Ssteam in the vapour phase. Alternatively, concentrated hydrochloric" ~" I- w* m j, B: I
acid can be reacted with the titanium-containing mineral to form a
: v% }) }+ q3 B7 E( Y' @7 Psolution of titanium tetrachloride, which is then further purified and/ {1 p# t, ]1 o6 h
converted to titanium dioxide by hydrolysis. The titanium dioxide is
; E2 O5 j5 O0 lfiltered, washed, and calcined.
* s2 {6 ]8 ?0 I9 E7 Z) p6 JCommercial titanium dioxide may be coated with small amounts of0 z( B m8 |& b- G# c7 R* a. g. f
alumina and/or silica to improve the technological properties of the1 w+ n, q- D" Y
product.9 h$ \7 f1 X: E* m/ f8 T! u
C.A.S. number 13463-67-7$ l' c6 ?4 S2 A: ?
Chemical formula TiO24 h, V% j, @8 f5 B D
Formula weight
- ]* i V3 p- \9 \* x g79.88
K9 m; s1 a# V* DAssay7 A" C' N, ~ Q. G. c; ~' X; b
Not less than 99.0% on the dried basis (on an aluminium oxide and
& d( p! ?) ]( i- _# K/ xsilicon dioxide-free basis)
* P8 O1 i3 |" A( N bDESCRIPTION0 M! z8 ]4 o0 O. l% Z
White to slightly coloured powder# Q; T' |6 m" J( Z
FUNCTIONAL USES
3 Z1 K3 K' ~. }, |4 lColour
2 ]+ ?, O# h* k3 @3 N7 ^% VCHARACTERISTICS7 Q5 g+ |! B5 D" _" q/ N
IDENTIFICATION! c. `& d8 ]3 X% \$ V/ h
Solubility (Vol. 4)
9 H4 q/ L: b- Y* L4 A' O/ _7 T6 QInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
' s. D% L) f; \% H( r3 csolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
& F1 `& ?5 h# S4 Wsulfuric acid.0 V" k2 U( ~: N m6 @
Colour reaction
. V+ P! [* M7 i7 v# m7 Q+ G8 \Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of% W& E' G: ~ }7 D
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
4 x; t2 f0 s: f% e4 v- A) Wwater and filter. To 5 ml of this clear filtrate, add a few drops of
, H! f1 X8 A1 ]hydrogen peroxide; an orange-red colour appears immediately.
+ |6 Y4 e/ Z/ _ P+ Z% S0 R; DPURITY
; K0 c1 \" z: L1 n7 \* ?2 l& d6 }Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)) t$ ^. V) H! @6 q$ c) ~
Loss on ignition (Vol. 4)3 Y5 a' ~ M- ?
Not more than 1.0% (800o) on the dried basis
4 X) Q( ?" {2 U+ S1 c" H, P( s. OAluminium oxide and/or
! T8 p: K" ~/ @3 {silicon dioxide
. j3 D! n# |7 T) ?+ t7 uNot more than 2%, either singly or combined* z9 O/ j- K. ~
See descriptions under TESTS
& w( S. w6 q$ o h+ KAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing ?, e" }0 h( F! r9 Y7 N0 B* P
alumina or silica.
$ p0 T# w& B3 O+ G- ?Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and4 n8 k+ }0 O; [/ R) B8 \2 m
place on a steam bath for 30 min with occasional stirring. Filter
- }# T1 j0 D7 O& W4 sthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
3 e7 p. F& ~9 Z$ V; S7 R0 Gwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the! P7 @) N' I8 _
combined filtrate and washings to dryness, and ignite at a dull red- y* _# b3 s1 m
heat to constant weight.
. Z/ S2 m" U2 [: m( }8 Z( lWater-soluble matter' \/ m4 H8 O: x- _; s
(Vol. 4)& w* o* m5 L. v9 g& Q# }. Z6 O6 H6 \2 w
Not more than 0.5%% J+ ^8 ^$ \5 V' y$ r
Proceed as directed under acid-soluble substances (above), using9 c" K n% W; U" k
water in place of 0.5 N hydrochloric acid.! q4 V* U% H0 w4 t
Impurities soluble in 0.5 N8 q: Q# M& n( l: N1 N" t
hydrochloric acid: J2 t7 K$ u, S% h6 v6 g( P
Antimony Not more than 2 mg/kg" B/ S2 O" p; B, \2 b6 Y4 z
See description under TESTS
( S. y. M4 h5 ^. d* o) VArsenic Not more than 1 mg/kg
c8 i q* p3 E: ?( |See description under TESTS
% [$ x: U3 `% g) E# D' VCadmium Not more than 1 mg/kg0 V/ J9 x, N' R* A' @
See description under TESTS
( f1 h0 f1 I# n: S" o6 eLead8 g8 d! t& ^ y" h. V8 K
Not more than 10 mg/kg- r4 a( `& [2 T) K6 d
See description under TESTS' h9 T# t. v2 l& V/ z# @, W( c. d) f! T
Mercury (Vol. 4) Not more than 1 mg/kg
: c: J; n8 G% H" U2 VDetermine using the cold vapour atomic absorption technique. Select a
! Z' ~% e ^9 e) g/ ^4 y5 I r& i# Zsample size appropriate to the specified level! E& [* t+ j2 b+ M7 E
TESTS
3 o; b1 a$ }9 Z/ V/ d; aPURITY TESTS. j8 t1 p4 k0 {
Impurities soluble in 0.5 N/ u" ~2 a7 A6 G9 n
hydrochloric acid
0 P; v7 F' H& [4 q+ [# U) QAntimony, arsenic,! r- X$ v- I0 H# X+ A/ \
cadmium and lead! }3 v/ |8 ~' Y& q' q; B
(Vol.4)
$ k, Z4 E2 d4 S8 W/ A; f7 b% GTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
5 ~% l" L7 a1 U# Hhydrochloric acid, cover with a watch glass, and heat to boiling on a
, L; U6 { j7 R7 [' m4 Chot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml3 Z' A7 q C& E# |4 ]* z2 C; _2 @# ]+ R
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
- D& C- @" C- W* j& `( X" w8 Mmaterial settles. Decant the supernatant extract through a Whatman
4 a3 R5 S5 @+ j5 J. P1 B7 UNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml$ r6 b& b3 @7 c& E2 d& ^& |# G
volumetric flask and retaining as much as possible of the undissolved9 X/ g5 `/ N' Z" p l7 B5 {: G
material in the centrifuge bottle. Add 10 ml of hot water to the original8 N! M" d+ G0 g4 }' x9 w) j+ n& x
beaker, washing off the watch glass with the water, and pour the
9 r$ w: M4 l& H% ^contents into the centrifuge bottle. Form a slurry, using a glass stirring
& H4 C: O/ n1 y; J n$ `. orod, and centrifuge. Decant through the same filter paper, and collect- |4 G: N2 O4 O# I
the washings in the volumetric flask containing the initial extract.9 V+ }0 C7 r: i% @+ `8 p0 r1 o$ x
Repeat the entire washing process two more times. Finally, wash the
" v% Z" y% }/ m" r2 gfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask7 T( W1 a1 X% ~& x
to room temperature, dilute to volume with water, and mix.6 j' `: [2 {& d8 ?
Determine antimony, cadmium, and lead using an AAS/ICP-AES( [' R _3 w4 V1 M: E( p! d+ Y; F
technique appropriate to the specified level. Determine arsenic using the
: [: I& L4 ^# Q `ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using+ x9 X' ]- b9 q& z
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than. p) N+ Y! t" C7 \+ v( J
1 g. The selection of sample size and method of sample preparation
. K, N, a0 ?) emay be based on the principles of the methods described in Volume 4.
9 w$ `. x) z: [' @* ?( o% ]6 v EAluminium oxide Reagents and sample solutions( \4 x* i, ]; R; m# ?* ?& e4 Q: @
0.01 N Zinc Sulfate p4 t4 n3 \0 X) @( e! b
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to$ \: j/ K* _1 D* k) f/ ?; m
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg# j8 V6 B, _$ p$ P
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
7 a3 z9 X9 {% [2 j' x5 m) s3 {concentrated hydrochloric acid, heating gently to effect solution, then
8 s3 y2 `2 Q8 b1 N9 E: Ytransfer the solution into a 1000-ml volumetric flask, dilute to volume
+ n0 T6 S) b( t* vwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500" V b! u) a7 }- y1 J" Q
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
/ P: b, ~# U) bconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
; L2 s$ V* `+ D$ |- H8 s0 w0 v25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
9 h0 p, E+ u9 j) K; D- ]/ tdropwise, ammonia solution (1 in 5) until the colour is just completely
. f& ~! r5 V5 o' r( w6 ]+ j: y. Qchanged from red to orange-yellow. Then, add:
2 h$ ]$ `9 d' f(a): 10 ml of ammonium acetate buffer solution (77 g of
" X; }$ e1 g* X9 u* M; a' Nammonium acetate plus 10 ml of glacial acetic acid, dilute to. b! L7 I* A) [
1000 ml with water) and7 H$ v0 P! M- \# h- Y9 }0 o
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
0 [) Z( E6 V& Xof diammonium hydrogen phosphate in 700 ml of water,
/ O7 I* J ~; z9 k9 Oadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
6 }1 F9 C/ b4 b7 j' |& Mthen dilute to 1000 ml with water).& ~- L7 r' E2 u* `! `. e8 r
Boil the solution for 5 min, cool it quickly to room temperature in a: i! B6 @( \) V+ _0 A9 v! c
stream of running water, add 3 drops of xylenol orange TS, and mix.# D$ G, e' ]0 D) ? D* w0 I
Using the zinc sulfate solution as titrant, titrate the solution to the first
" x' F p7 a) U! _ Wyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
6 r$ n% k0 x6 B) {; ]: G2 zThis titration should be performed quickly near the end-point by: g H9 \/ x: j) o. {3 q
adding rapidly 0.2 ml increments of the titrant until the first colour# H( ~4 _: z" E( D( M0 D0 }
change occurs; although the colour will fade in 5-10 sec, it is the true7 S4 `4 m& B4 q/ ~/ {
end-point. Failure to observe the first colour change will result in an
. K3 [. y. y# tincorrect titration. The fading end-point does not occur at the second1 E# e+ P1 d5 z. J
end-point.)
. o' G( k% o) pAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
* w2 B5 ]8 Y' G; q- T* B3 R) ~( Pstream of running water. Titrate this solution, using the zinc sulfate8 D' V( M& }3 U) l# [
solution as titrant, to the same fugitive yellow-brown or pink end-point
' [) C( r# C. Ias described above.
- G, D" N% o1 ~0 Q" N# lCalculate the titre T of zinc sulfate solution by the formula:2 p# N o1 j6 c2 ^2 b8 S1 f
T = 18.896 W / V
5 Z' x( l0 Y; c8 P& ^) Swhere% \; H( \# f5 `* {. |
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
, M" P* E- N0 d$ Q$ }- v- x. W0 cW is the mass (g) of aluminium wire" M# m! F6 Y9 X( F
V is the ml of the zinc sulfate solution consumed in the. w7 Y5 z) n J7 R0 W% Y
second titration9 f( @4 i) R3 }# n# |6 ?$ O2 U
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and' Q) c$ d. D2 E5 P2 C7 @0 `( @1 u, A! e# w
R is the ratio of the formula weight of aluminium oxide to H, S f) z/ {! s$ r
that of elemental aluminium.
% U7 H5 B3 S+ G [! H0 \Sample Solution A
. ]8 g5 _" [' \Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica/ G$ S6 F. h9 F( W$ W' P
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).7 K' k" T5 P" j& S8 F
(Note: Do not use more sodium bisulfate than specified, as an excess6 s' `2 _5 p v) Y7 ]3 Y2 b
concentration of salt will interfere with the EDTA titration later on in the
4 q: |( S# w4 R$ _6 j# |, @procedure.) Begin heating the flask at low heat on a hot plate, and: H# H0 d! {+ f$ Y" x% \
then gradually raise the temperature until full heat is reached.
5 u7 Q0 S2 W; X; Q! g(Caution: perform this procedure in a well ventilated area. ) When
0 I1 L+ f* n: n, A, d4 I/ bspattering has stopped and light fumes of SO3 appear, heat in the full
! u2 a0 ~2 D" v* a5 Tflame of a Meeker burner, with the flask tilted so that the fusion of the2 \6 l. i. G2 x6 u4 ]8 F2 L! l
sample and sodium bisulfate is concentrated at one end of the flask.2 z2 _" P) H* h' W$ O1 ]( M/ o4 ~2 \
Swirl constantly until the melt is clear (except for silica content), but
2 s# }# v; O. r# ~5 `/ Aguard against prolonged heating to avoid precipitation of titanium, Z2 E6 l/ b" F
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until9 {) E( A( Z6 P* y. p6 H9 ]
the mass has dissolved and a clear solution results. Cool, and dilute to: ~3 u6 Z# _& k6 |# E$ I
120 ml with water. Introduce a magnetic stir bar into the flask.2 h5 j/ a. z9 U# r2 v7 a
Sample Solution B
/ V5 g; L! \! g0 B. h$ }" k4 \: Y- tPrepare 200 ml of an approximately 6.25 M solution of sodium
/ {2 _3 V8 l% [* L0 j6 Mhydroxide. Add 65 ml of this solution to Sample Solution A, while
1 I% r4 Z0 {; i! sstirring with the magnetic stirrer; pour the remaining 135 ml of the4 O/ R6 J) X% |/ M' z" R" e( Q5 T
alkali solution into a 500-ml volumetric flask.- z6 K$ J q1 w# b" M" R
Slowly, with constant stirring, add the sample mixture to the alkali/ A- M, W+ T, x {
solution in the 500-ml volumetric flask; dilute to volume with water,1 h' m9 v4 x1 |* r
and mix. (Note: If the procedure is delayed at this point for more than' X( H# f5 B- L1 v0 A8 b6 y
2 hours, store the contents of the volumetric flask in a polyethylene/ O# y8 I! i7 n/ r: l
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),* L$ V8 x( C3 T6 [0 Q! p4 o* _& j
then filter the supernatant liquid through a very fine filter paper. Label" q7 p; p8 i7 V: n7 Z) u2 ]6 A
the filtrate Sample Solution B., B- T7 t4 x" l0 _0 v; |7 i
Sample Solution C. i5 j* Z* U( \9 V0 s/ p n7 D
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
) M& `! a+ A. d! ]6 d/ ~flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid) Z- _4 z @! V( k0 h, K# f
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
3 Q' G! p: W2 t( PM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
! w, m2 [ n$ G. T* v5 Tknown, calculate the optimum volume of EDTA solution to be added! b" Z" ? M0 }& z* L: w, h3 _
by the formula: (4 x % Al2O3) + 5.]
+ `3 |, B; b! @; U, b& d6 }6 a( SAdd, dropwise, ammonia solution (1 in 5) until the colour is just( X5 F6 H6 {4 A/ J, b4 l) _( A' f
completely changed from red to orange-yellow. Then add10 ml each) t: C8 I; `% x" n# n E0 b! n, @2 p/ Y
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
% i$ P3 R5 A. [; O& Lroom temperature in a stream of running water, add 3 drops of xylenol# U, A/ y+ I8 m5 Q
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
3 ~: f. L3 w- r/ F5 W( c3 sbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
/ M( b& c. R& i3 M6 xpH, a pink colour indicates that not enough of the EDTA solution has$ |3 c5 B7 M0 ?
been added, in which case, discard the solution and repeat this$ e! `4 q; T- p9 n% H7 m
procedure with another 100 ml of Sample Solution B, using 50 ml,0 b1 V1 S- Z! E; K$ S2 w( n' j
rather than 25 ml, of 0.02 M disodium EDTA.3 c* e0 u X0 [* q0 h' Q
Procedure
: C0 l" N% ^- O4 nUsing the standardized zinc sulfate solution as titrant, titrate Sample
: S; p; P* `0 M0 q" LSolution C to the first yellow-brown or pink end-point that persists for1 [2 D* y) S: l* a9 h; _
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
/ N; n% z$ P/ u# W+ v* Dtitration should require more than 8 ml of titrant, but for more accurate
. c1 S5 c. d; k% _1 F5 d0 Mwork a titration of 10-15 ml is desirable.
1 d6 w7 A* [. ]Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
7 l2 q& L: | o9 r" k( j3 [, zmin, and cool in a stream of running water. Titrate this solution, using6 I# `6 o9 C( Y( h( L
the standardized zinc sulfate solution as titrant, to the same fugitive. N) ^, O+ q. V. L, ?2 S
yellow-brown or pink end-point as described above.5 Q8 u" _6 z+ R$ x$ h
Calculation:
7 C. y t# e [6 ECalculate the percentage of aluminium oxide (Al2O3) in the sample4 k d: c" y* v* I" ]4 ~
taken by the formula:
5 s- g: S( i) J. A- ^7 G$ ^0 X% L% Al2O3 = 100 × (0.005VT)/S
W3 x) ^: l' pwhere2 i; F) w9 q0 I3 a+ B/ H$ ]: g* K
V is the number of ml of 0.01 N zinc sulfate consumed in
9 q) P! R p; e/ z; L3 T$ Kthe second titration,- O" q; r/ D1 [1 f9 Y
T is the titre of the zinc sulfate solution,+ A2 U+ x. h8 f) ^" o
S is the mass (g) of the sample taken, and) Y0 y4 N- `1 |
0.005 = 500 ml / (1000mg/g × 100 ml).
; |' e6 i. o8 Z0 C$ I- tSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica7 _' T' i% F' w& u! D
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).& G5 A; D7 i% j& v0 T& Y) E
Heat gently over a Meeker burner, while swirling the flask, until8 `' Q/ p& k) C; u$ X
decomposition and fusion are complete and the melt is clear, except- N; V. }( D) {( Q. D
for the silica content, and then cool. (Caution: Do not overheat the$ e- t2 D! N' L8 Z1 o
contents of the flask at the beginning, and heat cautiously during: \7 x0 D4 l. o4 Q4 _
fusion to avoid spattering.)0 h% K1 b9 l9 S4 I: `0 ^
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
2 F* ~) r" t( t7 d kcarefully and slowly until the melt is dissolved. Cool, and carefully add
; I# N- |3 p0 s" {2 ~150 ml of water by pouring very small portions down the sides of the
0 r$ ~$ z0 W8 M$ K, U8 Rflask, with frequent swirling to avoid over-heating and spattering. Allow
( G3 j2 R7 Z/ g) Q/ `+ w" _the contents of the flask to cool, and filter through fine ashless filter& {! E f; a, s$ g" u' n1 h: H
paper, using a 60 degree gravity funnel. Rinse out all the silica from
+ i6 a) e' s4 othe flask onto the filter paper with sulfuric acid solution (1 in 10)." V- H: G$ U# D8 i: }
Transfer the filter paper and its contents into a platinum crucible, dry in/ V4 Z1 d: `% w( P
an oven at 1200, and heat the partly covered crucible over a Bunsen
2 c! x, l8 R, x' ?1 {+ A- Gburner. To prevent flaming of the filter paper, first heat the cover from" v' a! J6 x. d
above, and then the crucible from below.( ]- y3 S4 k4 \- I( B
When the filter paper is consumed, transfer the crucible to a muffle
1 ?9 w9 n3 Q/ Z, s$ n: Mfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
; L$ h1 f) h/ V5 q( z0 h* A% Oweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated2 b" s G d' G. | x
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first* t( j. T# V- c5 q8 i# h! j _
on a low-heat hot plate (to remove the HF) and then over a Bunsen
! Z7 D! L2 L8 _5 y% Hburner (to remove the H2SO4). Take precautions to avoid spattering,# i: G; b8 _9 q% `
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a& b5 [ r5 q+ O
desiccator, and weigh again. Record the difference between the two, e3 U# m. l/ [8 h3 L1 x/ P1 l
weights as the content of SiO2 in the sample.
1 z% L7 a$ {6 V2 @7 |2 OMETHOD OF ASSAY8 U# V/ C$ S; }# b1 v/ Z3 \5 m; Q4 k
Accurately weigh about 150 mg of the sample, previously dried at 105o
: h3 L% t& p j- hfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water N! e7 W' j& L. i
and shake until a homogeneous, milky suspension is obtained. Add 30. E6 l: q6 n. r9 U H
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially. t+ k& S8 d- Z1 t+ L2 U1 I
heat gently, then heat strongly until a clear solution is obtained. Cool,9 p/ O+ G; {# C3 n; }; H
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
' |+ M0 {% N; u) d8 q9 f* |acid, and stir. Add 3 g of aluminium metal, and immediately insert a0 f* k9 X7 }4 b$ q
rubber stopper fitted with a U-shaped glass tube while immersing the( {' X4 H. r& G/ J
other end of the U-tube into a saturated solution of sodium
1 E. R) R2 O9 c8 Vbicarbonate contained in a 500-ml wide-mouth bottle, and generate$ I( w4 e4 \! O; h
hydrogen. Allow to stand for a few minutes after the aluminium metal
! r$ z; |; P- T' D- |has dissolved completely to produce a transparent purple solution.1 y* T( |+ Y; U. c, s. G, Y
Cool to below 50o in running water, and remove the rubber stopper
$ J& R3 s$ h! Mcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
1 R# |& n/ t' O/ w+ q& Y% @, S! \solution as an indicator, and immediately titrate with 0.2 N ferric
$ v3 H( G" P' y" H- Uammonium sulfate until a faint brown colour that persists for 30
: X3 J1 ~" }0 m a7 _- lseconds is obtained. Perform a blank determination and make any
, J$ Q) \$ C5 ~! v: K; C4 fnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
: A W; f( [ q/ T6 `# ^" _equivalent to 7.990 mg of TiO2.
Y' n* |+ u3 f a- s4 j |
|