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二氧化钛(钛白粉)
二氧化钛(钛白粉)1 i- L F9 S5 n& {: V! R9 A8 _* ~ _
g# G/ y* J4 b0 _
JECFA关于二氧化钛(钛白粉)的结论% t p" [1 s" A) R; Z2 [! \: {
8 F9 Z2 G/ E- P7 t
摘要: 2006年JECFA关于二氧化钛的结论
/ G. d+ z4 ~6 } _3 j" eADI值:不作限制。
! J% y$ _% f8 l功能:着色剂: K$ R; W' G" P9 q+ ^& S: P; _; D
0 J+ A: O, t$ `5 O
TITANIUM DIOXIDE
/ t) ?. J8 L1 u" b; A* H0 IPrepared at the 67th JECFA (2006) and published in FAO JECFA
! f2 {9 a1 [+ ]; H. D6 ?* ^" VMonographs 3 (2006), superseding specifications prepared at the 63rd+ m: Z' R0 h N# x4 n& r
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the5 M; ^# Q9 ^3 d% N
Combined Compendium of Food Additive Specifications, FAO JECFA" ^; J* K d7 E3 g$ u" O6 S. r& R3 f7 K
Monographs 1 (2005). An ADI “not limited” was established at the 13th: k0 B6 r2 J8 a2 _" p$ {6 {
JECFA (1969).5 ^/ F8 N: w' O) ~
SYNONYMS m8 j4 h' x: u/ i# q5 Q& b
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
; P1 O& C9 C5 ~DEFINITION0 T' ], }3 s6 {: j) w _/ x9 Q* ~
Titanium dioxide is produced by either the sulfate or the chloride5 {( n ^/ @/ X% j6 o
process. Processing conditions determine the form (anatase or rutile
. i7 a+ N# H+ a3 K1 R6 Mstructure) of the final product.
8 z( ^( o# J$ C2 d2 vIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)$ _5 Y7 ?& n* M; h/ c% x% q2 I9 s
or ilmenite and titanium slag. After a series of purification steps, the3 p% ?/ R: g; O5 I9 T
isolated titanium dioxide is finally washed with water, calcined, and
7 ?8 v8 j9 `5 J& m$ Xmicronized.
+ }' \- K- p( n$ i( E8 \In the chloride process, chlorine gas is reacted with a titaniumcontaining- c% a! n) F F6 i/ n5 e
mineral under reducing conditions to form anhydrous$ _% C7 c; i( \: ?4 u
titanium tetrachloride, which is subsequently purified and converted to
7 S% T! A" a: `, z2 Atitanium dioxide either by direct thermal oxidation or by reaction with
( ~$ h7 h9 X8 P4 Zsteam in the vapour phase. Alternatively, concentrated hydrochloric
) C# T% G# j2 X+ ~: Racid can be reacted with the titanium-containing mineral to form a/ h* s: c4 c) D% \2 D+ f
solution of titanium tetrachloride, which is then further purified and
+ N% S5 g2 B. u7 ?% n# M0 aconverted to titanium dioxide by hydrolysis. The titanium dioxide is
/ d3 Q+ |7 q& x' y% j. \1 Rfiltered, washed, and calcined.
' m: f) B& O Z5 l, k: PCommercial titanium dioxide may be coated with small amounts of
* ]' X( M1 e8 b, Z; _alumina and/or silica to improve the technological properties of the
6 q0 X w ?7 [2 qproduct.3 x7 {; _; Y% N6 ^& O v1 w$ k/ x
C.A.S. number 13463-67-7* G6 E F2 B3 H2 O
Chemical formula TiO2
5 b0 L) K; R8 Z/ x4 XFormula weight
9 U# x# g! l0 y, B& F- r79.88& r# x6 h$ f9 V z6 v- l8 |% X
Assay! W9 l" x1 M; [. g: k1 M. } @
Not less than 99.0% on the dried basis (on an aluminium oxide and! A w- n' x7 l6 k; b
silicon dioxide-free basis)
7 b1 [" j+ Z! K3 V vDESCRIPTION: c$ g5 O, u1 y
White to slightly coloured powder& S4 ^/ k" O7 y3 I8 R+ h( C, Y
FUNCTIONAL USES
9 _' z# y, E* J8 z) ]3 {; M+ FColour6 i$ `1 ^/ g( A- v0 t
CHARACTERISTICS
5 T5 ~, T' Z3 ?1 HIDENTIFICATION
# j9 n4 {! h) w, A. R( O$ pSolubility (Vol. 4); Z5 p. ?* E: v. z1 \: H1 z
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic4 p# {. `9 t Y( }# q. ]
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
: e& X# b) o; \! `) O7 Csulfuric acid.
Q. k9 m, a+ P7 g# Q& y% Z" FColour reaction7 f# J- q) M0 O
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of; I: S% T7 Q$ ^ x, G
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
. ~! r0 k u4 \: Zwater and filter. To 5 ml of this clear filtrate, add a few drops of/ n& B5 B4 H$ g8 l& r: D
hydrogen peroxide; an orange-red colour appears immediately.
( X; r3 a1 s& M6 Q+ CPURITY
% }. n0 v" x- L7 }, h! `Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)- h' E. ^' g2 a7 m
Loss on ignition (Vol. 4)4 y; g8 c) y8 @7 l0 w: e; E! B
Not more than 1.0% (800o) on the dried basis* W; n7 p, ~/ N5 k
Aluminium oxide and/or
' `* ^- y/ b8 H+ x$ Q* H8 ~5 i$ Isilicon dioxide" F" b# N$ d- l
Not more than 2%, either singly or combined5 n: g9 \7 N$ T; X
See descriptions under TESTS
7 P; C8 F$ w6 Q/ M7 t6 H+ oAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing' M' y8 O' b5 e8 s% N1 g
alumina or silica.
3 ]+ A% }( G# a6 E1 ySuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
2 X; [% {+ I. [" D% A/ Vplace on a steam bath for 30 min with occasional stirring. Filter
) J3 C7 P" j w4 ?6 N! gthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
5 { t a: j4 P, ^. M, pwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the) Y( r* W2 J% t9 z/ L5 Y% C
combined filtrate and washings to dryness, and ignite at a dull red9 g7 T) N, w% z. o
heat to constant weight. v( [1 G- V# F3 Q( T; ^& u% K
Water-soluble matter
1 T0 |. ~# Z3 s+ `- V' Q' D(Vol. 4)7 R/ w$ b( n- s+ ]! H1 f9 F
Not more than 0.5%) N$ F% L3 i7 _+ o2 C8 ]
Proceed as directed under acid-soluble substances (above), using+ k2 P' }5 @6 T, j# C
water in place of 0.5 N hydrochloric acid., a' @" O) ~$ d/ \8 ~
Impurities soluble in 0.5 N
2 y* _4 u) W) B3 {hydrochloric acid1 |5 G2 U. M9 l! j
Antimony Not more than 2 mg/kg
( _- D. S" e) Y" t: XSee description under TESTS v1 a, I+ L! `
Arsenic Not more than 1 mg/kg
+ B4 X/ _- E- ZSee description under TESTS6 G* ^! q! a" D" J8 `- D% e
Cadmium Not more than 1 mg/kg" i! r+ z( T0 K5 L' A' d8 }; k
See description under TESTS+ Y; N+ p/ U+ B5 B+ x9 j% \ ?2 D
Lead- d7 n) g0 r7 j5 i
Not more than 10 mg/kg! g% s, ~ B! t G
See description under TESTS
% `8 O2 W" ~2 g7 UMercury (Vol. 4) Not more than 1 mg/kg+ N! t, W* p0 q v' n9 V* `
Determine using the cold vapour atomic absorption technique. Select a9 A6 |! R) x6 g" x- f
sample size appropriate to the specified level
" @) a" l8 y. F- J3 e, ]/ mTESTS8 A7 \. [# d+ ~! E- _% w
PURITY TESTS" u9 A) ~* ~4 q0 ^. o' M7 x
Impurities soluble in 0.5 N) |) I# c, k3 H; E0 w
hydrochloric acid
& W/ X7 m1 [7 CAntimony, arsenic,6 t+ S5 ?; U$ T1 {. I, q$ u
cadmium and lead
1 G* F, C1 v2 N# T: L9 S0 Z3 x8 Q(Vol.4)
H) }; o' |- Z& B# h/ C) c3 GTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N: L6 G4 j( u7 l; j& T
hydrochloric acid, cover with a watch glass, and heat to boiling on a
: i! ^0 g) L5 L; V# n, thot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
8 E2 p, i5 q9 u$ g: B# Lcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved6 ]6 H4 W% y9 R; T
material settles. Decant the supernatant extract through a Whatman) t" M! q5 e6 d7 ^
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
7 U! H4 Q( b) S# O5 C1 E- `volumetric flask and retaining as much as possible of the undissolved' V- R% w7 c5 x3 {, a& O
material in the centrifuge bottle. Add 10 ml of hot water to the original
9 A7 w m* h+ \7 |6 a( C# a' N! abeaker, washing off the watch glass with the water, and pour the0 {1 `3 f1 W6 a" U( ]
contents into the centrifuge bottle. Form a slurry, using a glass stirring. Q* _$ d) b% R0 H/ ~- ]/ R
rod, and centrifuge. Decant through the same filter paper, and collect1 Z, D+ N6 ?: d: I" e" v
the washings in the volumetric flask containing the initial extract.
* P% |* V$ ?4 C4 S9 F% _, ]% M2 GRepeat the entire washing process two more times. Finally, wash the) o$ \; m; e# a" [. L6 b8 a
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
1 c m# r: B: p2 M5 B! kto room temperature, dilute to volume with water, and mix.
' M8 b& K$ k! \: u' c% kDetermine antimony, cadmium, and lead using an AAS/ICP-AES/ H6 M7 ^( s! Z3 g b% O
technique appropriate to the specified level. Determine arsenic using the
) J/ l& \: V* m R/ y9 t4 UICP-AES/AAS-hydride technique. Alternatively, determine arsenic using; d+ g6 o" n4 [, Z# D
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
4 @0 {3 a+ ~* t7 }8 i2 C1 g. The selection of sample size and method of sample preparation
9 p* d! _1 W8 E" ~5 ^" mmay be based on the principles of the methods described in Volume 4.6 b( E+ `# M4 W: v1 Z" Y
Aluminium oxide Reagents and sample solutions4 I o+ U% s$ Y0 N! V1 [ M1 A
0.01 N Zinc Sulfate- B# C+ M" q) `* L$ ], t% j; _
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
# X9 j$ ]* Z& p; b% @* n8 \make 1000 ml. Standardize the solution as follows: Dissolve 500 mg5 @( W. Z3 f ?5 r3 q# a
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
: f0 G' @0 C/ Y& n1 o7 zconcentrated hydrochloric acid, heating gently to effect solution, then: P0 v! a* K% O4 ~. ?
transfer the solution into a 1000-ml volumetric flask, dilute to volume
* V T0 x2 s! h9 j$ Y) t6 a' ^* owith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
; v! ?1 ], ^9 D2 p$ P$ n+ g' F4 B4 w lml Erlenmeyer flask containing 90 ml of water and 3 ml of8 M9 l( B k; I C' A3 _% z
concentrated hydrochloric acid, add 1 drop of methyl orange TS and9 Q* H% Y3 d: D% B
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,. q- Y, `$ A1 _* z$ I2 y7 }7 ]
dropwise, ammonia solution (1 in 5) until the colour is just completely! E5 E* F- y9 m, P$ l9 r
changed from red to orange-yellow. Then, add:% y! W- N) b) | t0 R" Y- H
(a): 10 ml of ammonium acetate buffer solution (77 g of
+ N" ?/ S/ k8 O c6 Mammonium acetate plus 10 ml of glacial acetic acid, dilute to
$ C9 x" h, J* F" G/ x4 F) p1000 ml with water) and* x7 i9 L( r( x t9 E' l8 ^5 u
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
$ i' U, L! I# U8 S4 R! ~+ Cof diammonium hydrogen phosphate in 700 ml of water,
& Q* x: v) N% r( i- ~% u+ Eadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,4 R) k& ?- S4 m- Q
then dilute to 1000 ml with water).
. F9 M8 g& E0 l5 KBoil the solution for 5 min, cool it quickly to room temperature in a
! o- ]' J8 E! e; ]6 Wstream of running water, add 3 drops of xylenol orange TS, and mix.
' O( v0 i6 @! KUsing the zinc sulfate solution as titrant, titrate the solution to the first( D8 V3 s. k7 N1 y. W
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
; I" d! C# @1 n6 D9 k* IThis titration should be performed quickly near the end-point by
0 _8 R' q& \2 Z0 v) L# `; yadding rapidly 0.2 ml increments of the titrant until the first colour
" U1 V# j7 x+ W8 u, e8 Pchange occurs; although the colour will fade in 5-10 sec, it is the true; l7 n' A. f1 ^& t/ G' }
end-point. Failure to observe the first colour change will result in an6 k' w0 }5 b# i
incorrect titration. The fading end-point does not occur at the second. r* [+ U; w# U: o' U
end-point.)- {, U( A, T+ U* V/ n
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a3 E- g7 [7 W' ?' V+ }) U% V
stream of running water. Titrate this solution, using the zinc sulfate
% B' j4 N! z% y3 m/ v# ^' zsolution as titrant, to the same fugitive yellow-brown or pink end-point
7 y$ W+ t/ ~' ]4 W" N- eas described above.( G" T6 q1 H C/ c
Calculate the titre T of zinc sulfate solution by the formula:
6 @. A) |5 e! N; W x- _2 h6 R$ Q& |T = 18.896 W / V# w ^( W" }# `% `
where4 o) C* J4 E0 |8 ^9 ~
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
7 ^0 P8 C' Z4 m5 ~1 l6 FW is the mass (g) of aluminium wire
$ g- T. M; i% f, T6 QV is the ml of the zinc sulfate solution consumed in the9 K8 |( u0 v: M$ v2 q$ p
second titration
6 _" p1 w! l6 j; @; \8 ~; t: h2 v18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
* T; A. _5 s# d TR is the ratio of the formula weight of aluminium oxide to
' m6 S2 a# w+ Q$ Vthat of elemental aluminium.3 N3 y% M" D5 P+ E T
Sample Solution A
: l: t' f9 W2 _4 XAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
# f3 F) k9 @; Wglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
1 T' I; g* |* \0 ? f4 g(Note: Do not use more sodium bisulfate than specified, as an excess
% a( p3 ~) ?7 ~1 z& fconcentration of salt will interfere with the EDTA titration later on in the
* R O9 y0 y8 z3 K5 X- O E7 F- K$ [9 Pprocedure.) Begin heating the flask at low heat on a hot plate, and
' P- h4 O& j, H$ ^* Wthen gradually raise the temperature until full heat is reached.
1 a0 l H- A8 C+ c(Caution: perform this procedure in a well ventilated area. ) When
( I) y, A Q. N( zspattering has stopped and light fumes of SO3 appear, heat in the full, ]0 F! t& B" `8 @. ?. z) C
flame of a Meeker burner, with the flask tilted so that the fusion of the' n8 ]$ _- h3 o/ G' n* L- ]( i- [
sample and sodium bisulfate is concentrated at one end of the flask.
' \" ?% } F$ v& QSwirl constantly until the melt is clear (except for silica content), but! c7 A5 z3 G( z. D" m9 s. N5 p
guard against prolonged heating to avoid precipitation of titanium
/ R ?; I3 e9 O5 c* Ddioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
* T! C0 @7 f* E: K: Kthe mass has dissolved and a clear solution results. Cool, and dilute to0 v7 o2 w0 {" m! y8 N
120 ml with water. Introduce a magnetic stir bar into the flask.$ f; N& }5 q3 }9 z0 f
Sample Solution B* o4 j7 Q3 t( {$ Y+ P. O; h
Prepare 200 ml of an approximately 6.25 M solution of sodium
; G& ?6 L2 |5 s) ]) vhydroxide. Add 65 ml of this solution to Sample Solution A, while
. U' u) R1 @' f- I j1 xstirring with the magnetic stirrer; pour the remaining 135 ml of the! O, K! C3 Q; @3 x1 c
alkali solution into a 500-ml volumetric flask.9 @# @0 I; p9 k. d4 I0 j; o
Slowly, with constant stirring, add the sample mixture to the alkali/ W2 J+ X( I! m& A) s
solution in the 500-ml volumetric flask; dilute to volume with water,. a0 y1 R6 u3 @
and mix. (Note: If the procedure is delayed at this point for more than0 Y7 _' ~8 l& g, J, \9 Z [& P/ Z& u
2 hours, store the contents of the volumetric flask in a polyethylene
: e1 [9 I9 H# I# ~bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
* f* z) n+ u1 pthen filter the supernatant liquid through a very fine filter paper. Label# ~# |# k) l3 U
the filtrate Sample Solution B.
: K! p0 T7 b, V0 K1 eSample Solution C
4 D7 z! w% V% d! U/ BTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer% [5 [6 A' m) s: K5 w1 M
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
" g6 e" k X1 e4 ]+ A: q# Usolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
$ ` c! C) R4 R! q o/ k5 W& dM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is$ h) r5 j4 @5 Z# ~$ r& k; p, i( ]) d' @8 ^
known, calculate the optimum volume of EDTA solution to be added: T, h2 V9 f4 b' i. L$ `5 I
by the formula: (4 x % Al2O3) + 5.]
7 I+ w+ e2 _$ ^2 `Add, dropwise, ammonia solution (1 in 5) until the colour is just
7 o# n" v) l+ U( J5 ycompletely changed from red to orange-yellow. Then add10 ml each6 e& E6 J: B$ A* w
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to; x& P" L; m3 \0 n& D
room temperature in a stream of running water, add 3 drops of xylenol
' T6 @+ ~3 V2 G3 F6 `/ Jorange TS, and mix. If the solution is purple, yellow-brown, or pink,) [3 l6 U) l6 |/ J& l
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired1 g1 i) S1 \! [7 E3 W" z; q& \
pH, a pink colour indicates that not enough of the EDTA solution has
, t% z8 _ X6 Y( k( ]8 s# rbeen added, in which case, discard the solution and repeat this
$ W; l) M, ^ ~" oprocedure with another 100 ml of Sample Solution B, using 50 ml,' K6 r- U, Z. n2 I0 v0 _, o
rather than 25 ml, of 0.02 M disodium EDTA.
; R0 ^9 k0 {- T" B5 U8 YProcedure
7 Q* N6 l' W$ MUsing the standardized zinc sulfate solution as titrant, titrate Sample
# e \( M |$ E- {* fSolution C to the first yellow-brown or pink end-point that persists for% E7 b2 k; _- o
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
3 V6 C' z. p8 ?) Etitration should require more than 8 ml of titrant, but for more accurate! `+ L$ Y! i1 \- m+ V1 X1 P
work a titration of 10-15 ml is desirable." t( w5 }( S( l. i2 n) f X; a
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
, \# v8 N* U& |min, and cool in a stream of running water. Titrate this solution, using" B/ a) S5 Q' x" v C1 M. E' i
the standardized zinc sulfate solution as titrant, to the same fugitive) z3 }1 Q2 z* Q3 A& X( u5 j" V
yellow-brown or pink end-point as described above., c7 e" e+ h- C
Calculation:
5 c4 V3 o+ B# W$ B& B4 O( oCalculate the percentage of aluminium oxide (Al2O3) in the sample8 O0 [/ L5 d. d/ ^% F+ j
taken by the formula:/ |6 G2 N' A3 c( X( F' T
% Al2O3 = 100 × (0.005VT)/S+ f# H* p, b" [- r K' K
where' }6 \" v9 g1 ?
V is the number of ml of 0.01 N zinc sulfate consumed in
" I2 R' P9 S. P2 y, Z* kthe second titration,6 @$ @: F' Y$ K# y4 |- T8 x$ D' W
T is the titre of the zinc sulfate solution,8 q; d, p' d( |6 A3 R" c0 \
S is the mass (g) of the sample taken, and- N2 C3 i( B1 ^% k6 W8 @
0.005 = 500 ml / (1000mg/g × 100 ml).
0 h: z/ k. ], {. O: e& iSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
8 a$ ^1 Z, K' p2 i! {8 J1 ]! l- wglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
" _' C1 C8 Y8 J% u Q% Z) E, kHeat gently over a Meeker burner, while swirling the flask, until, e8 C" B) | U2 c
decomposition and fusion are complete and the melt is clear, except
! [ w: a8 w; I/ m+ {4 T. i2 e; Gfor the silica content, and then cool. (Caution: Do not overheat the
5 }8 b8 A% s' {8 T: hcontents of the flask at the beginning, and heat cautiously during
: b& ^/ m' B6 j! zfusion to avoid spattering.)
% {+ Z" p7 ^1 W5 {To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat6 C4 W$ {! W' s1 [
carefully and slowly until the melt is dissolved. Cool, and carefully add
* @) r+ ^' v/ g; `) p& u. M m150 ml of water by pouring very small portions down the sides of the$ q8 i! ? i+ |& b7 t
flask, with frequent swirling to avoid over-heating and spattering. Allow- V2 E3 E0 O; P4 {6 E7 }
the contents of the flask to cool, and filter through fine ashless filter) Z* n% S$ m8 B7 i0 e8 C N
paper, using a 60 degree gravity funnel. Rinse out all the silica from- U! |" i- X. R
the flask onto the filter paper with sulfuric acid solution (1 in 10).4 d4 r# n: w* H4 [' C3 d
Transfer the filter paper and its contents into a platinum crucible, dry in3 c* s8 E1 h8 c+ c* h
an oven at 1200, and heat the partly covered crucible over a Bunsen, S3 ^9 _/ D5 e* h
burner. To prevent flaming of the filter paper, first heat the cover from$ ?& G& W6 c9 [" I: ^6 c3 T9 Z
above, and then the crucible from below.: E: U! o5 N: k) R
When the filter paper is consumed, transfer the crucible to a muffle% R) a9 Y- M- W# G6 ~0 W
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and8 Y5 O1 d" [ w4 ~9 p
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated) {4 r+ k# x6 N
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
; K2 k+ t% X" ]6 O, v" a) U" ron a low-heat hot plate (to remove the HF) and then over a Bunsen
# |% D# @# c0 n' b: _6 E; g9 ]5 nburner (to remove the H2SO4). Take precautions to avoid spattering,3 K' S% h" y6 x P9 [0 k; r3 f2 u
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
/ p% R' U }& `, c1 Q0 rdesiccator, and weigh again. Record the difference between the two
, y, k6 X- _0 @9 T' l, @weights as the content of SiO2 in the sample.
7 ]: K5 A: E2 @METHOD OF ASSAY( a: L# }8 ?* O/ O
Accurately weigh about 150 mg of the sample, previously dried at 105o
) U6 {% P4 y! d9 s% ifor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water. B/ k- [. D a5 f# A- f
and shake until a homogeneous, milky suspension is obtained. Add 30' f3 T1 c3 [9 B" G) w. X
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
. [8 K. U' h$ rheat gently, then heat strongly until a clear solution is obtained. Cool,; z e* t: z# b* r7 c" X. i
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
* I5 v- @* M4 Y: `- a1 Oacid, and stir. Add 3 g of aluminium metal, and immediately insert a
3 J/ k4 x$ [" {. C2 [rubber stopper fitted with a U-shaped glass tube while immersing the3 J( G* [9 |8 n' w$ X2 m
other end of the U-tube into a saturated solution of sodium
( k( J; F- S) Gbicarbonate contained in a 500-ml wide-mouth bottle, and generate# K1 F( K @: C: {9 B
hydrogen. Allow to stand for a few minutes after the aluminium metal
- B) a- d+ z+ `$ G7 u- o l8 `0 hhas dissolved completely to produce a transparent purple solution.1 C- X- b; h6 Q$ d
Cool to below 50o in running water, and remove the rubber stopper3 T, V- `$ J) y5 d7 z: m
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate) E! C3 p6 Y# Q6 a- g
solution as an indicator, and immediately titrate with 0.2 N ferric; P ]+ g7 L3 t1 ]4 T5 I
ammonium sulfate until a faint brown colour that persists for 30% }# d$ I! u* r( f% \0 X Z3 e
seconds is obtained. Perform a blank determination and make any
! r4 j! X! ^1 I7 C( O6 vnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is0 s- g8 Y: v3 s0 x1 X) X
equivalent to 7.990 mg of TiO2.( U7 C) ~' b% d7 I
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