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二氧化钛(钛白粉)
二氧化钛(钛白粉)
% H. l+ F9 Q: f7 x- U+ P. F" T3 j/ k0 U6 v+ B
JECFA关于二氧化钛(钛白粉)的结论) c$ W" {7 h8 l; {
V0 h7 y1 Y4 H! _& S/ C; H
摘要: 2006年JECFA关于二氧化钛的结论
# k" H8 Z, W! L6 v* o1 M$ B+ F: eADI值:不作限制。. Y9 F% b! f" o; _( m
功能:着色剂2 F( P, c" v4 w7 v
. S# u$ K! O& g2 ?9 `4 sTITANIUM DIOXIDE
# x3 s/ X# m6 ^! ~2 N, H1 s+ X% [Prepared at the 67th JECFA (2006) and published in FAO JECFA
~7 c7 U8 b0 M. a0 V W( p( @4 M6 Q, N- iMonographs 3 (2006), superseding specifications prepared at the 63rd. X* R, R( g F u: Q8 ]* Y
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
8 l& j: D1 I/ z3 p/ @5 yCombined Compendium of Food Additive Specifications, FAO JECFA
. m) E$ Z0 n# z, u/ I( NMonographs 1 (2005). An ADI “not limited” was established at the 13th* v. J& x8 B+ ~% a- }0 C: `
JECFA (1969).
& B: j1 u0 T9 |0 V9 |SYNONYMS
/ O! H! a/ Y; v' c: E: h1 B, dTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
. P, F }& K. |DEFINITION
/ P( a, C1 f ?0 E! vTitanium dioxide is produced by either the sulfate or the chloride3 J! ]& z1 `, b3 v7 w
process. Processing conditions determine the form (anatase or rutile
7 W, W ~( M/ ?) ^* P0 Dstructure) of the final product. _9 }: G! [6 Q0 H; b5 @- W
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
5 \ @/ a& X$ d: o& ]- C5 Oor ilmenite and titanium slag. After a series of purification steps, the
$ m* ?, x7 O) a1 T1 }isolated titanium dioxide is finally washed with water, calcined, and
9 v5 l9 h2 y: n2 umicronized.
6 v+ _' n) g$ N qIn the chloride process, chlorine gas is reacted with a titaniumcontaining
, ?# Q! M* ]5 J2 f9 N" f5 Bmineral under reducing conditions to form anhydrous
% c1 `$ `! M; W# ptitanium tetrachloride, which is subsequently purified and converted to/ H1 @) y# {5 S+ O' ?, i
titanium dioxide either by direct thermal oxidation or by reaction with
. T# ^' }1 Y$ Wsteam in the vapour phase. Alternatively, concentrated hydrochloric
! f. {) s: Q1 k/ {; r. z- o: o6 ]acid can be reacted with the titanium-containing mineral to form a
# f# `; q+ X$ H/ m- _: Xsolution of titanium tetrachloride, which is then further purified and
+ h- C7 `1 B- [2 nconverted to titanium dioxide by hydrolysis. The titanium dioxide is
3 s# c& N* }2 R Pfiltered, washed, and calcined.
1 p( S3 a: p4 ^: q7 E2 VCommercial titanium dioxide may be coated with small amounts of
6 u3 Y7 j) [* a8 g5 V v8 }' Falumina and/or silica to improve the technological properties of the
* A% s. F/ s3 ^$ ]- [% Cproduct.0 X& q6 V3 t1 f- q' C4 Z5 J
C.A.S. number 13463-67-7
6 T& t* w* E3 P3 kChemical formula TiO25 Z& J; r% t* s9 G+ O) ~. b( k( _0 ^! l
Formula weight+ A5 v4 D/ w* f2 ?
79.88
4 b+ k# {/ F9 n0 `Assay
! h8 h. I5 g& \9 RNot less than 99.0% on the dried basis (on an aluminium oxide and
_3 P( d1 g& f5 t. ~+ ^- i4 x W# s& ^silicon dioxide-free basis)
+ w# D& j5 K# B% T$ E% e' YDESCRIPTION
3 G, i% B; `$ b0 \White to slightly coloured powder
' F9 ~) s! P7 M& MFUNCTIONAL USES) Q, k) D& t b T z
Colour8 F6 X: H* N& J% [0 d% q
CHARACTERISTICS! P$ a2 @; \: [3 j( H. `
IDENTIFICATION4 d: w2 V. P2 Y+ `* Y+ B$ A1 v9 Q4 G
Solubility (Vol. 4)
6 t# m5 F; o. V6 C; }4 P0 RInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic( q' z. F7 @ h/ o W, X; E
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
- D0 F1 m! x0 h. q' J- ~) U) dsulfuric acid.! B" y9 }$ Q6 a) a: G: p6 G: m
Colour reaction E9 t. v! T+ u8 x+ Q6 B2 V# C
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of5 q" r. r z2 _5 C9 r2 V
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with2 I, @( Z" v0 q3 g: d
water and filter. To 5 ml of this clear filtrate, add a few drops of" d& {0 e& |# s. [' v- x9 W, U
hydrogen peroxide; an orange-red colour appears immediately.
. s! f ]/ k9 ^6 {5 y2 D R( j1 pPURITY6 _2 j% S. Z9 b. f
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
/ L' J8 c: x1 R5 C, B' h" yLoss on ignition (Vol. 4)
8 g W* n4 Z8 JNot more than 1.0% (800o) on the dried basis7 d2 p8 `+ h7 p7 F) N
Aluminium oxide and/or+ C/ @2 c" Y2 m
silicon dioxide; x, c6 O m: K6 s* o
Not more than 2%, either singly or combined# ]) B9 l' s+ X9 D7 N8 L1 a
See descriptions under TESTS
6 g% M* I8 z* o) C$ [Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
* B' G$ w$ q7 g9 | Falumina or silica.: p) f2 v5 s1 K8 j
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
+ |% i& S% F; J/ e# S( d% x: t2 Iplace on a steam bath for 30 min with occasional stirring. Filter, h z! V4 I3 u+ s% | y8 |
through a Gooch crucible fitted with a glass fibre filter paper. Wash: Q% @- A- r5 H$ |& \% k D
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
h: _' h; z# q. s/ Hcombined filtrate and washings to dryness, and ignite at a dull red7 S4 D6 } Y+ z. I+ z: e. k
heat to constant weight.
% \' S) r' Q0 X7 I. PWater-soluble matter
3 c s Q/ ~( B0 l6 {5 _(Vol. 4)/ m" I% j. e7 r& ~# U3 o
Not more than 0.5%) z4 y, S1 n6 z; l
Proceed as directed under acid-soluble substances (above), using. K/ T% T1 h0 d
water in place of 0.5 N hydrochloric acid.
( {4 J \, s3 u% e$ zImpurities soluble in 0.5 N
8 |8 s% }& E* ^9 O3 p( zhydrochloric acid' ~6 S1 S# O; s) D! |1 T! H3 k0 ]
Antimony Not more than 2 mg/kg
0 n% h1 U7 W9 Z: nSee description under TESTS
- s& p8 c: H1 W* e& H. _: cArsenic Not more than 1 mg/kg$ `1 u# f5 c- x8 Y' v
See description under TESTS
/ G2 a9 K- O& j0 X5 b, ECadmium Not more than 1 mg/kg
( P2 k" `) {* r+ ^6 V# t3 j5 QSee description under TESTS, Z3 E+ G9 n3 m& T
Lead/ |' j, H, z; C
Not more than 10 mg/kg8 y7 W5 R9 S1 ~& y* [9 f! {" P
See description under TESTS
~+ w7 A! R% V3 I& C5 U/ G5 RMercury (Vol. 4) Not more than 1 mg/kg
5 b$ M% e! }2 a9 MDetermine using the cold vapour atomic absorption technique. Select a$ G' g4 c# k, r1 W
sample size appropriate to the specified level
* s% |8 w; Y9 k& [& T8 k- Y4 r4 _TESTS4 W$ c7 x3 |! c" d7 c" h
PURITY TESTS. F2 f1 S& S' Z/ g
Impurities soluble in 0.5 N# @2 G7 h5 k' A7 N* o
hydrochloric acid2 J. \/ J1 `7 _) Z/ j
Antimony, arsenic,
; N( @/ `7 h$ } w- F3 G2 ycadmium and lead
$ q/ t" z, |8 a ] t5 E(Vol.4)
' r& E6 m$ E' a) ~Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N# P. z Z5 v! Z: v& D: a, F; Q
hydrochloric acid, cover with a watch glass, and heat to boiling on a
2 ~* w/ w( u2 W% s4 p9 ~hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml7 H. a& D9 V. i# C- O
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
- P0 l Q6 ^8 ?) ^7 H ~% tmaterial settles. Decant the supernatant extract through a Whatman4 E! c! U. d1 i& y9 E
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
; ~$ Z# z# @; Z6 ~* u2 [* Jvolumetric flask and retaining as much as possible of the undissolved
/ l( ~% g' u! K7 bmaterial in the centrifuge bottle. Add 10 ml of hot water to the original Z; {9 m- P9 }/ L0 U
beaker, washing off the watch glass with the water, and pour the
7 ]6 u* t8 g4 g8 Z. a5 m7 B& Q0 f. |contents into the centrifuge bottle. Form a slurry, using a glass stirring# |3 k$ k3 {' u0 M
rod, and centrifuge. Decant through the same filter paper, and collect1 E w" _5 d# k& ]
the washings in the volumetric flask containing the initial extract.
3 S. z4 K# W" M& uRepeat the entire washing process two more times. Finally, wash the
" c+ X% A" o% K& F' c3 S# Xfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
7 e* M; h. Z# ]5 Lto room temperature, dilute to volume with water, and mix.9 T X7 Y; _1 k X
Determine antimony, cadmium, and lead using an AAS/ICP-AES
0 N: J, Y* Z; {4 v7 J1 z ^4 U; |& G7 k `technique appropriate to the specified level. Determine arsenic using the
: R. G. U* E' [/ V' f" _ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
# l) o% {' x5 f$ Q4 pMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
0 x+ e/ B$ f' W) C- q, H" m8 \1 g. The selection of sample size and method of sample preparation
Z) e& B/ Q) R' E' {may be based on the principles of the methods described in Volume 4.
3 ^2 i6 x* ?! S( OAluminium oxide Reagents and sample solutions
- @' l8 l- B. j' M+ Q) L3 \- O0.01 N Zinc Sulfate
, x; l' D; {' G6 t5 U: u: C, WDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
+ D8 z2 b) ~8 S7 t# n3 vmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg% B9 {5 P! P/ n; h# c& E5 o6 M
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
9 l+ f% Y# _# fconcentrated hydrochloric acid, heating gently to effect solution, then
5 W" o" r* R* H5 ~transfer the solution into a 1000-ml volumetric flask, dilute to volume
9 f. u b u$ D# W; ~with water, and mix. Transfer a 10 ml aliquot of this solution into a 500, L# a! f% S: k2 p# ~) d4 P% H
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
u: x8 ?7 E2 ?; ^8 Gconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
]! ]( f1 J" A8 ~" L# ^0 R, S1 T25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add," e3 d' G; }' g
dropwise, ammonia solution (1 in 5) until the colour is just completely
" J6 ~7 b2 p; S) I7 Wchanged from red to orange-yellow. Then, add:
, \+ I8 W, S" R" s3 ?9 B5 z' c' g- J. `(a): 10 ml of ammonium acetate buffer solution (77 g of
( s( I+ F/ W7 U7 N q7 Lammonium acetate plus 10 ml of glacial acetic acid, dilute to
/ r. P0 [* j/ u$ \- `/ |) e1000 ml with water) and3 l& W+ n2 P, p) @
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
+ ~% ^/ X2 F1 J( ]of diammonium hydrogen phosphate in 700 ml of water,
/ q8 i& T3 q( T) e# o& Iadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,2 d8 Q3 g* R* e" x
then dilute to 1000 ml with water).
( x" B9 O k$ @% s. F4 B$ R3 a3 HBoil the solution for 5 min, cool it quickly to room temperature in a
( ~: L/ J5 E: [stream of running water, add 3 drops of xylenol orange TS, and mix." x& j, g. @) X# N! i- c( e
Using the zinc sulfate solution as titrant, titrate the solution to the first
3 Q# Q, [6 v) e( ~* iyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:2 S: p5 x) J" I- s
This titration should be performed quickly near the end-point by
) L1 S+ Y5 y- K9 X5 `; X" w j+ eadding rapidly 0.2 ml increments of the titrant until the first colour
( [1 u7 }- v* {; kchange occurs; although the colour will fade in 5-10 sec, it is the true
% \2 Z& ]* z# C2 n" xend-point. Failure to observe the first colour change will result in an" b5 a% U6 q2 l+ f6 G
incorrect titration. The fading end-point does not occur at the second
. s" Q4 [" b4 a) q' {9 O0 zend-point.)
1 }* S9 Z! L; ? f2 ?, X. h8 uAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
9 o4 D5 X! f( I$ P7 v- Astream of running water. Titrate this solution, using the zinc sulfate
1 w1 n1 H% i3 G* w8 D2 k3 K' ]solution as titrant, to the same fugitive yellow-brown or pink end-point
" Q& L4 P4 E' n) Y2 nas described above.
) z& h/ X, S" [% j& |7 O& _Calculate the titre T of zinc sulfate solution by the formula:8 N, c' p, W6 f% k2 _
T = 18.896 W / V
k, N l7 T! o* Zwhere6 s) e3 b7 R1 w1 K r- K
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution. n M. H ~% V& c- F7 k/ s+ n
W is the mass (g) of aluminium wire
; E0 N$ {" b+ G. k \. tV is the ml of the zinc sulfate solution consumed in the
# r7 C0 G. x% C1 ~; Z( Dsecond titration
! R8 L9 |) u& x* x) D4 k7 Y18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
% t8 r; H4 V1 @R is the ratio of the formula weight of aluminium oxide to0 \; u. D0 h( _, R5 ?
that of elemental aluminium.0 q/ I; }3 T0 X# {" b
Sample Solution A
. u# K5 `. g1 y# K! |Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica: j* O* d5 T* @) j
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
3 k! M- U1 Z8 g0 `. T! y(Note: Do not use more sodium bisulfate than specified, as an excess
# V. R. ?/ v! F% e: E+ tconcentration of salt will interfere with the EDTA titration later on in the$ p# f( V; S. v/ C- }& i% f1 Z
procedure.) Begin heating the flask at low heat on a hot plate, and% e! m$ @2 z- O7 Z# n
then gradually raise the temperature until full heat is reached., m1 W4 X, F6 D) N7 R+ h8 Z
(Caution: perform this procedure in a well ventilated area. ) When
( z+ H1 p. ^( N. o; e/ K, @spattering has stopped and light fumes of SO3 appear, heat in the full
" v% @8 m, J/ P4 i0 oflame of a Meeker burner, with the flask tilted so that the fusion of the
+ D6 S5 a6 }( N1 q0 ksample and sodium bisulfate is concentrated at one end of the flask.
" k* _2 ~( a2 KSwirl constantly until the melt is clear (except for silica content), but
; `) \) n$ z5 Oguard against prolonged heating to avoid precipitation of titanium0 C N; y6 l6 t! p- K
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
9 [3 C! z7 r# O- ]9 ~# g9 }the mass has dissolved and a clear solution results. Cool, and dilute to
3 q6 K9 W" b4 h0 u) w1 L120 ml with water. Introduce a magnetic stir bar into the flask.
3 Y$ m/ _& H$ I- L& n( h( @+ ASample Solution B
% J& S) p$ O1 e5 [, P( \Prepare 200 ml of an approximately 6.25 M solution of sodium
/ ? l2 r4 L+ g }hydroxide. Add 65 ml of this solution to Sample Solution A, while4 z$ J( y# r$ R# ^6 U g- \9 o
stirring with the magnetic stirrer; pour the remaining 135 ml of the
, u/ L1 O- w: c2 M% Valkali solution into a 500-ml volumetric flask.* |. P3 J" j6 Z' I* D( r
Slowly, with constant stirring, add the sample mixture to the alkali
( V, h, c( b: I H3 Bsolution in the 500-ml volumetric flask; dilute to volume with water, J1 o6 S: ~1 }1 S
and mix. (Note: If the procedure is delayed at this point for more than, n- |% _! ?% B
2 hours, store the contents of the volumetric flask in a polyethylene
?1 |. X: k( C/ E( `8 m2 nbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
9 e" X" s* @. c# X% O+ ithen filter the supernatant liquid through a very fine filter paper. Label0 _- N: J6 Z1 O6 ]! A4 q: x
the filtrate Sample Solution B.
: K+ u- m. i6 U) b' R ?Sample Solution C
* U5 b' w! o( I- s, A3 o CTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
/ f; O) `- ?; |. h& W" h* c, U) {flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
5 ^% o$ v/ n+ Y% ~4 C3 g: fsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
2 Z+ a* a4 d$ E% ?2 r# q# ZM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
. @1 M; }3 K) _ \& l7 F ^known, calculate the optimum volume of EDTA solution to be added
" N$ \7 {) A2 E8 S, dby the formula: (4 x % Al2O3) + 5.]
! G G# R4 [- J$ K# UAdd, dropwise, ammonia solution (1 in 5) until the colour is just
% G$ Z( }! \4 g$ h; m3 J% `: Vcompletely changed from red to orange-yellow. Then add10 ml each
; p# u$ P2 T- [. {5 C) @of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to# k+ K6 @, ?- r5 M$ C, k y
room temperature in a stream of running water, add 3 drops of xylenol8 ]+ z* g) _# _7 `
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
3 |6 J& V6 f/ ~* m$ Ebring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired" n. D7 H0 y2 i# j6 j
pH, a pink colour indicates that not enough of the EDTA solution has
2 F' l$ _& B' b* d0 e6 f) Kbeen added, in which case, discard the solution and repeat this! [2 K6 ^8 J4 s+ K4 H+ u% f
procedure with another 100 ml of Sample Solution B, using 50 ml,7 X1 R" R$ L! J% g. D
rather than 25 ml, of 0.02 M disodium EDTA.
& |9 Q9 D+ \0 r+ F' m- nProcedure3 s" i, X, C8 f6 B
Using the standardized zinc sulfate solution as titrant, titrate Sample
) a, q" s7 _ o. v2 e$ PSolution C to the first yellow-brown or pink end-point that persists for3 ?! A8 k, n& ?$ ~
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
a( o% t$ d9 B# o* D! E9 Z! Ztitration should require more than 8 ml of titrant, but for more accurate, T8 P" u9 g5 F0 G( F
work a titration of 10-15 ml is desirable.
! g- p. b0 I4 L0 a9 YAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
c% r6 O" K; x0 z, u7 X3 I [min, and cool in a stream of running water. Titrate this solution, using; X# r! F* p0 j" g: f J
the standardized zinc sulfate solution as titrant, to the same fugitive8 A0 l U! D* I. o0 J
yellow-brown or pink end-point as described above.$ K6 ]6 `3 _6 s: E, A5 I
Calculation:6 u/ l9 \9 H3 w$ m# g4 v
Calculate the percentage of aluminium oxide (Al2O3) in the sample, H1 u0 S7 d) T2 y
taken by the formula:' X: m) z" Q8 X- J, U4 e9 O3 B+ F
% Al2O3 = 100 × (0.005VT)/S" m( Y- H2 C F
where5 v% Q7 b0 [& r! B) u& @
V is the number of ml of 0.01 N zinc sulfate consumed in
7 U" _ `( x7 Nthe second titration,
9 n3 k. u$ e; q1 ET is the titre of the zinc sulfate solution,
. A( i/ H( n; ]S is the mass (g) of the sample taken, and
6 [0 \# }2 w5 b$ ^* j1 @$ C% y& Y0.005 = 500 ml / (1000mg/g × 100 ml).
& ?6 V6 y/ U9 _9 oSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica+ w/ [5 { r5 i2 Z7 u9 W
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
K; J) b! u; B% e0 @- x( CHeat gently over a Meeker burner, while swirling the flask, until
, A/ W7 C8 O, k8 Mdecomposition and fusion are complete and the melt is clear, except0 _# z1 y( V6 C Y$ u! ^! Q# m
for the silica content, and then cool. (Caution: Do not overheat the
7 H, d4 ^1 a/ v; \- w' c6 {% Wcontents of the flask at the beginning, and heat cautiously during
& m9 x( D4 t& I0 Ufusion to avoid spattering.), Q3 M; }4 U: o( K- a
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat) y* O5 x) h! J: ~ w5 M
carefully and slowly until the melt is dissolved. Cool, and carefully add
& F+ f/ W# ]0 v" n% r3 g2 i150 ml of water by pouring very small portions down the sides of the
1 S6 u0 {. l0 \0 v, Iflask, with frequent swirling to avoid over-heating and spattering. Allow
5 k5 C! V$ V Ethe contents of the flask to cool, and filter through fine ashless filter7 d y( |6 u5 |7 ^, d7 V
paper, using a 60 degree gravity funnel. Rinse out all the silica from E! X' L$ q$ u# _8 T* X* E3 w, r
the flask onto the filter paper with sulfuric acid solution (1 in 10).% Y6 ^, g5 u1 u7 P+ Q
Transfer the filter paper and its contents into a platinum crucible, dry in) o/ u# q8 d2 O5 o2 e5 M$ {, }
an oven at 1200, and heat the partly covered crucible over a Bunsen& M' b+ |& v7 ]- x+ v5 _" R+ ~
burner. To prevent flaming of the filter paper, first heat the cover from
' e' {6 {6 i0 U2 babove, and then the crucible from below.9 N& Y& l2 k1 u4 Z ?
When the filter paper is consumed, transfer the crucible to a muffle3 ]) O, _$ ~9 R8 ]* v ?
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
1 e! ]9 B1 N, l. Z! t- uweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated, F4 I' M/ I. O- n4 D
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first* Z/ w7 [% u) O. O
on a low-heat hot plate (to remove the HF) and then over a Bunsen# q* j0 s( `1 a x# y# p
burner (to remove the H2SO4). Take precautions to avoid spattering,1 O4 P4 B3 T: V$ h- m4 O
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a; Q3 C. Y$ b4 `6 u( z
desiccator, and weigh again. Record the difference between the two' V0 {7 @( J( E1 z. D Q
weights as the content of SiO2 in the sample.
9 s6 V4 z. G5 B4 u+ b9 ZMETHOD OF ASSAY
% m, J( w% M+ \$ I; v* X, ~' q3 K( RAccurately weigh about 150 mg of the sample, previously dried at 105o
5 R( l8 K# g7 ~) ?for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
! `5 X" R% }: d% w5 D& p7 d3 J" z3 Pand shake until a homogeneous, milky suspension is obtained. Add 30! ]# V% k: r9 ]0 ?1 [3 h
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
, v- \5 j6 l* v# O& d4 ]/ [heat gently, then heat strongly until a clear solution is obtained. Cool, I% E8 k3 A! D" l
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric% q' _- n% M% |9 y( M- K
acid, and stir. Add 3 g of aluminium metal, and immediately insert a; \, ~; P4 G' k$ W6 G* U9 Y
rubber stopper fitted with a U-shaped glass tube while immersing the. ^) g& W# w7 M# N6 G4 ~" i( O
other end of the U-tube into a saturated solution of sodium
: Z& z; ]6 H% S0 Dbicarbonate contained in a 500-ml wide-mouth bottle, and generate
# X7 f2 m6 |' Lhydrogen. Allow to stand for a few minutes after the aluminium metal& S9 w* y* | j/ V
has dissolved completely to produce a transparent purple solution.+ W/ o. h9 [+ N' C" C& d
Cool to below 50o in running water, and remove the rubber stopper" y$ v( J; T6 V+ T. E# f, F( F
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate! U9 L% g" ^. }
solution as an indicator, and immediately titrate with 0.2 N ferric
5 X% p ~) n9 E# ?4 X2 Nammonium sulfate until a faint brown colour that persists for 30
1 U' H, D8 s: N& Q s$ B! oseconds is obtained. Perform a blank determination and make any
4 U: i8 O R$ p0 x2 e1 w4 }; Gnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
) Y4 t7 b6 ^7 e2 _% Mequivalent to 7.990 mg of TiO2.* l6 ?/ H9 f& v' t4 V9 g
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