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二氧化钛(钛白粉)
二氧化钛(钛白粉)
# r6 b/ B* p4 }, a0 O$ i# h9 C8 `+ C' E, l
JECFA关于二氧化钛(钛白粉)的结论
' V x. @. N* k8 x/ _
5 ?- F: @1 n; h$ j, D! m W摘要: 2006年JECFA关于二氧化钛的结论
. X' E! H* {' P" }ADI值:不作限制。3 l2 d+ B' [) K9 y W
功能:着色剂
' V4 P+ I) B+ l4 z6 [3 @2 d- k+ I- s# M' L* J# }" j! U7 j* f
TITANIUM DIOXIDE
4 o3 c$ U9 S! F1 n, FPrepared at the 67th JECFA (2006) and published in FAO JECFA8 T0 e7 x* a6 p9 H/ m
Monographs 3 (2006), superseding specifications prepared at the 63rd
. p+ Y( J8 l9 P. K" |# AJECFA (2004) and published in FNP 52 Add 12 (2004) and in the: g) `# ^5 S6 a/ L4 H" _) j ^6 t
Combined Compendium of Food Additive Specifications, FAO JECFA1 c( r2 A, f1 ^0 K! n) s, t
Monographs 1 (2005). An ADI “not limited” was established at the 13th1 o$ v/ _# `( f0 b. Q$ ]
JECFA (1969).9 a% e. Q* V" {/ S" A
SYNONYMS& x @9 `, \% z* i- g
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171# |" M, N1 V& y, y1 U$ M
DEFINITION
1 n# K1 l! R6 D. u+ QTitanium dioxide is produced by either the sulfate or the chloride {- T5 ^- ?; t& |5 G- v$ `
process. Processing conditions determine the form (anatase or rutile
; i0 `5 C# l7 o# ?% u, o( o( B$ gstructure) of the final product.
5 z* x/ R* F2 A2 J3 dIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)8 ^1 e- [( l) H
or ilmenite and titanium slag. After a series of purification steps, the
( _) `& [7 B; G- w$ Z+ iisolated titanium dioxide is finally washed with water, calcined, and
5 K2 B9 Y( H0 jmicronized.
5 F8 h8 m) u" N \+ ?In the chloride process, chlorine gas is reacted with a titaniumcontaining7 L- L6 b b I0 R6 y4 o' l6 f* n; x
mineral under reducing conditions to form anhydrous+ M2 L! v4 U! ?. [$ Z/ X( A5 T
titanium tetrachloride, which is subsequently purified and converted to2 f7 D2 j/ {2 _9 _' Z
titanium dioxide either by direct thermal oxidation or by reaction with
* }+ u' C: l/ B J0 ]) b" `* Q2 L$ Hsteam in the vapour phase. Alternatively, concentrated hydrochloric" M& Y/ E& e# B5 @2 R9 W. Z
acid can be reacted with the titanium-containing mineral to form a( |3 V5 I3 y1 ~, S2 I7 {
solution of titanium tetrachloride, which is then further purified and! |5 ]( e+ ]* O2 i0 J" |7 H( I+ ]
converted to titanium dioxide by hydrolysis. The titanium dioxide is
6 g4 u* F- w0 x( k1 T+ Q2 bfiltered, washed, and calcined.) F+ i6 w- v/ k+ p8 b+ \* }
Commercial titanium dioxide may be coated with small amounts of# P3 @- K- z2 z8 d; g2 p
alumina and/or silica to improve the technological properties of the# C* j t( s2 h/ x. v# G' a
product.
1 i: {# @. I7 V, a5 h, K! u9 uC.A.S. number 13463-67-7; L$ U* K7 I6 E+ K5 b5 G
Chemical formula TiO2
0 Q/ F7 Q+ g/ d3 D3 ^+ [; k2 dFormula weight: D! f" ^7 z* o {" Q. Y! C
79.88
4 _0 ^$ A" }1 \4 S( y" y2 R1 cAssay
5 J# }8 w; I" U3 {& FNot less than 99.0% on the dried basis (on an aluminium oxide and
7 i! G' P" ^7 Y% Z7 L# z$ Fsilicon dioxide-free basis) v7 k% _, _4 Y+ e8 U/ f
DESCRIPTION
; ?+ l1 M* O2 o6 q2 M* QWhite to slightly coloured powder
- w0 `( w' [9 [ E+ V* F, XFUNCTIONAL USES
( u6 I) {3 b. H9 O+ Q& q+ `& HColour
3 F9 o) w6 K0 {* [CHARACTERISTICS: G, X5 D* c4 K9 c
IDENTIFICATION9 [, C+ M3 A) P$ E
Solubility (Vol. 4)
/ G' q2 U1 g- I% [) |/ Y; d& LInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
! C: t5 C9 `; m8 L7 ~+ Z/ T2 ]: \' csolvents. Dissolves slowly in hydrofluoric acid and hot concentrated0 m4 L" _" j- @/ z
sulfuric acid.: y! E2 p$ {2 K5 T) n, P6 K& l
Colour reaction
2 W5 h+ \! M7 ?, h& W+ X( jAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of+ O' } I+ `5 C6 I0 _
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with+ V& v' a' n3 w3 d! O$ u
water and filter. To 5 ml of this clear filtrate, add a few drops of
5 ~8 M# U& \! N' H8 U$ y) fhydrogen peroxide; an orange-red colour appears immediately./ G$ S# c8 ? U( F- Q E$ W8 f0 }4 i
PURITY3 y# S" j3 p% {+ | d
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
) ~ G3 Q" _* Z1 FLoss on ignition (Vol. 4)9 @9 C7 u; ]3 U1 m. e) e
Not more than 1.0% (800o) on the dried basis ^ J& N3 g" `4 T; U. _
Aluminium oxide and/or3 j- G& x' S5 l. z1 y$ A; J9 G; R
silicon dioxide' N* y1 Q) R$ ~! D' [
Not more than 2%, either singly or combined* w$ O* R6 ~# v: c3 F
See descriptions under TESTS. o, {6 ?6 ~1 f$ M
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
' q7 X2 C( M( galumina or silica.6 U. m5 _4 z$ I; p/ B' Z
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and% F, M# I& J0 Q" x2 j
place on a steam bath for 30 min with occasional stirring. Filter
. k2 |4 [* U/ B' ~through a Gooch crucible fitted with a glass fibre filter paper. Wash8 I; p8 K, p# G G) m
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
/ O) r9 @, v6 ?3 Z3 E5 G" w# Ucombined filtrate and washings to dryness, and ignite at a dull red- `" k3 V* r: u; r
heat to constant weight.7 L& _/ b+ Y. D0 Z1 v9 m
Water-soluble matter
6 O- x: i2 n) D9 O(Vol. 4)/ y5 r# ` _2 e0 d L N/ C! g0 F9 v
Not more than 0.5%- v6 T! `2 P+ _5 G1 ^, N D0 l
Proceed as directed under acid-soluble substances (above), using
# G0 v% U8 \9 iwater in place of 0.5 N hydrochloric acid.& a3 A+ o; x7 l- V. D
Impurities soluble in 0.5 N6 Z2 `' R6 K, _. q# X3 E0 _
hydrochloric acid7 |8 H- o3 ^+ r4 z
Antimony Not more than 2 mg/kg ]2 T& G7 Q/ T! ^% Q; G# V( d
See description under TESTS
4 M/ X% X/ t# |3 [( nArsenic Not more than 1 mg/kg
; C* J; ^/ V: B) n' lSee description under TESTS
; ?$ ^" ?7 d/ R2 D' v5 x( kCadmium Not more than 1 mg/kg( c! K; Y6 z9 ^3 r. v' u/ a
See description under TESTS2 g7 n/ {+ F& \# E4 N l* A" v; R& ]
Lead6 E6 O4 F6 ~! v" f
Not more than 10 mg/kg
* p2 o+ p1 H5 q. J, m# ~See description under TESTS
* C( x% ?& p' x" {Mercury (Vol. 4) Not more than 1 mg/kg
: m( a: O' S( J$ UDetermine using the cold vapour atomic absorption technique. Select a7 g9 Z8 a# } V* e R
sample size appropriate to the specified level/ W/ [! ]3 u) e1 T- u
TESTS
i* M4 f$ `6 RPURITY TESTS) Z" {4 U: r" v" _) Y/ d
Impurities soluble in 0.5 N
( }4 _/ v/ R3 o9 qhydrochloric acid5 ]8 E# g/ a. [$ y! `6 k
Antimony, arsenic, a- [, R% Y# b& J1 o. w
cadmium and lead1 J* `0 {( E/ V( i* s
(Vol.4)
& P- o# x+ e( F) `6 L) j, YTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N$ k3 V# L/ o* s0 V# N
hydrochloric acid, cover with a watch glass, and heat to boiling on a- k# k# c% Z, p6 v; _! x6 `; E
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
- P" l4 t" x" `centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
8 z( s: T: [6 W4 n' V% Y" Pmaterial settles. Decant the supernatant extract through a Whatman* e& t5 `# L4 c! C& r% Y
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml2 u; G& }$ I S0 _, P
volumetric flask and retaining as much as possible of the undissolved; [4 e* h( | R& u* M: r
material in the centrifuge bottle. Add 10 ml of hot water to the original+ X0 N" a' |, I. S( F
beaker, washing off the watch glass with the water, and pour the F6 M6 F) K3 G4 ~
contents into the centrifuge bottle. Form a slurry, using a glass stirring5 p. T% u( S8 J& |0 E
rod, and centrifuge. Decant through the same filter paper, and collect
- i' i- o8 a# {: `4 `) @the washings in the volumetric flask containing the initial extract.
$ G, E+ a, ~; l: y( XRepeat the entire washing process two more times. Finally, wash the
D3 A) K! f9 w0 L! Gfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
* J' K$ K/ q' |( K1 i- ?" kto room temperature, dilute to volume with water, and mix.
1 l' r* |, S% bDetermine antimony, cadmium, and lead using an AAS/ICP-AES& C# Z2 _! \9 X/ I/ k- t
technique appropriate to the specified level. Determine arsenic using the
: A/ J& C( v% S# GICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
) y/ R5 ?4 G* W! C4 `. j8 @2 }Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
$ @: ~, P1 ]8 ?( j7 c1 g. The selection of sample size and method of sample preparation
; E4 p1 b6 j! j g+ }may be based on the principles of the methods described in Volume 4.. v( O* R: j( I# D8 H
Aluminium oxide Reagents and sample solutions
0 K m3 }+ \5 b/ }- l- D0.01 N Zinc Sulfate' z6 `' ?% x4 ~7 _
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to& A" k# _7 g' c6 j" h
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
& g- D# s: Y7 [' X' \3 @8 hof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of) V# t% [9 R; u/ O
concentrated hydrochloric acid, heating gently to effect solution, then
7 x/ D' r- a; _3 O2 E% T! ]+ dtransfer the solution into a 1000-ml volumetric flask, dilute to volume
% ~& e; K' K+ rwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
% E3 e5 N* i, z8 m: t$ T+ o% sml Erlenmeyer flask containing 90 ml of water and 3 ml of* `, y* q5 X9 f) N( d
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
' v( V0 Z7 f/ D- l# @5 {25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
- B% z Z, i8 P# n \' c9 Zdropwise, ammonia solution (1 in 5) until the colour is just completely
" @% S2 X. H; p7 Cchanged from red to orange-yellow. Then, add:2 W7 A1 ] ]6 [, W( ~% j/ y
(a): 10 ml of ammonium acetate buffer solution (77 g of
/ I: I/ h' A- R0 Y; [/ V+ B) v* D6 Yammonium acetate plus 10 ml of glacial acetic acid, dilute to
( U8 B0 D/ q r9 n$ G1000 ml with water) and/ e* _& p8 D" K4 A: z! x
(b): 10 ml of diammonium hydrogen phosphate solution (150 g0 [ k9 y" w5 p2 l
of diammonium hydrogen phosphate in 700 ml of water,
. q# U; E$ { n! u" cadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid, u1 @# i+ F+ V3 F9 o6 D
then dilute to 1000 ml with water).% x& S& ~$ F0 b1 D, l, f3 l) J- a
Boil the solution for 5 min, cool it quickly to room temperature in a
2 Q1 p( r/ O s) S/ Estream of running water, add 3 drops of xylenol orange TS, and mix.
8 X0 Z0 r& e( T a7 rUsing the zinc sulfate solution as titrant, titrate the solution to the first
5 M: _8 M$ m( a2 g1 m4 H+ [yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
8 L5 q4 `% g1 CThis titration should be performed quickly near the end-point by% @5 V& Y/ S1 N& L5 Z, |- F/ {, R
adding rapidly 0.2 ml increments of the titrant until the first colour
. V8 |* B e) o0 R2 N6 `. Gchange occurs; although the colour will fade in 5-10 sec, it is the true
- y8 ^. ]7 u( zend-point. Failure to observe the first colour change will result in an; a: h- p& b ]" B
incorrect titration. The fading end-point does not occur at the second
& W2 E+ ?- O! F- ?: {0 ~8 Jend-point.)
0 _; O$ A+ J. [% oAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a( k3 T* h* z3 E! }! ?
stream of running water. Titrate this solution, using the zinc sulfate9 N; F# \. v" g3 D3 U' h
solution as titrant, to the same fugitive yellow-brown or pink end-point, n+ w& \1 }( H3 |
as described above.
+ G1 j( H* A: ~! ~/ VCalculate the titre T of zinc sulfate solution by the formula:7 Q1 q7 r. k* o7 q2 Y& m6 k* D' Z
T = 18.896 W / V
% C5 M( d7 @# uwhere: W, G1 p7 m/ r2 k/ y6 U. T0 |" u
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution: p- n0 t# J* e
W is the mass (g) of aluminium wire
~: Q( j3 v. \* M3 W+ U+ h2 }; @V is the ml of the zinc sulfate solution consumed in the& L& A& N5 `2 u% i$ }$ @
second titration
6 Q" x- m d! T18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and6 E$ L( f+ b( ^
R is the ratio of the formula weight of aluminium oxide to r, ?; W2 Z$ ` l: G% c
that of elemental aluminium.
( p: C0 V; m5 V/ sSample Solution A
' ?$ z0 G4 ^5 p% x8 }3 LAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
9 N' ^" s+ E O: g" }9 fglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
# u' N/ @: a/ R$ T(Note: Do not use more sodium bisulfate than specified, as an excess
8 ]: p( p( e |) l( E3 A5 Jconcentration of salt will interfere with the EDTA titration later on in the' R( Z* G4 k) j
procedure.) Begin heating the flask at low heat on a hot plate, and) p# Z8 |7 t% |/ D
then gradually raise the temperature until full heat is reached.) g* o, n5 _7 W$ |+ n, f
(Caution: perform this procedure in a well ventilated area. ) When' I' I5 r- n! ]8 u
spattering has stopped and light fumes of SO3 appear, heat in the full+ [/ r( u7 L3 H7 Z+ C- V! M
flame of a Meeker burner, with the flask tilted so that the fusion of the
. F6 z. l1 V- ]) |sample and sodium bisulfate is concentrated at one end of the flask.6 Z/ ]. {0 b! `0 {( Q0 F+ l; J
Swirl constantly until the melt is clear (except for silica content), but% R; }# `0 |8 A) X0 t
guard against prolonged heating to avoid precipitation of titanium5 C. Q a* L; b' h/ Y' Y* L
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until3 X% o2 F. z$ x8 _' X: U
the mass has dissolved and a clear solution results. Cool, and dilute to
9 q( ?" X+ `. {3 v120 ml with water. Introduce a magnetic stir bar into the flask.9 k2 g6 z8 s2 P5 `9 |" ~/ ?
Sample Solution B* M+ Z" ~& P0 ?* i8 ?9 A
Prepare 200 ml of an approximately 6.25 M solution of sodium
5 q5 ]4 G: G/ E" @: a3 \, I$ L/ Vhydroxide. Add 65 ml of this solution to Sample Solution A, while, `: w5 J, h8 k3 K8 l p
stirring with the magnetic stirrer; pour the remaining 135 ml of the
" H" i9 w G& Q/ E* }( Ralkali solution into a 500-ml volumetric flask.6 f( t g2 N0 K9 M9 C% G# d
Slowly, with constant stirring, add the sample mixture to the alkali
# L& [; {) c. t- I0 esolution in the 500-ml volumetric flask; dilute to volume with water,
# R, O7 I9 ]3 Z9 Uand mix. (Note: If the procedure is delayed at this point for more than, o* r* X# i, S
2 hours, store the contents of the volumetric flask in a polyethylene
7 T: z9 v, w: ^! _) gbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),2 F' v; a+ s4 V& K
then filter the supernatant liquid through a very fine filter paper. Label: F c! ]* T/ x% o# ~) r3 j
the filtrate Sample Solution B.8 L; N8 n$ @7 o' w9 i5 B& `7 d
Sample Solution C4 L9 `" p4 q* `: _3 T
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer0 b* [$ x! |- ^8 k5 e$ j
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
; F# A& G) p3 n6 y& Rsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02, S( ^1 S; ~7 l
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is& ^ }- e* @7 z: J4 y! a \9 l; A8 r
known, calculate the optimum volume of EDTA solution to be added
9 q5 n' b# _) dby the formula: (4 x % Al2O3) + 5.]
6 X. ^' e4 r; J1 A3 H$ p% DAdd, dropwise, ammonia solution (1 in 5) until the colour is just
- ~1 q; Z% F9 B: m2 T v7 Icompletely changed from red to orange-yellow. Then add10 ml each {4 E% Z5 H. c. o3 m
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
3 E+ M% a9 {. b; Oroom temperature in a stream of running water, add 3 drops of xylenol$ P3 R: c- S# N
orange TS, and mix. If the solution is purple, yellow-brown, or pink,. w2 ~) M9 i* q
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
/ h- v" C3 v$ {, xpH, a pink colour indicates that not enough of the EDTA solution has
7 p8 i5 x- ]3 G3 N% Dbeen added, in which case, discard the solution and repeat this a) w( D$ v1 q5 m
procedure with another 100 ml of Sample Solution B, using 50 ml,
6 _; i( A; p6 ~( A/ l7 p" S9 Zrather than 25 ml, of 0.02 M disodium EDTA.3 V& t# n* l- }$ g+ j2 d
Procedure
1 |) ]7 q$ t8 V y; gUsing the standardized zinc sulfate solution as titrant, titrate Sample8 b( Y* h4 o+ H0 a% `% [
Solution C to the first yellow-brown or pink end-point that persists for" c& v \1 V# J; K& O
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first) d0 g5 q3 v! A6 ^0 w) O6 ]) l) N) @
titration should require more than 8 ml of titrant, but for more accurate
+ r3 ], w* h/ Dwork a titration of 10-15 ml is desirable.. e" L. C ]4 r! A2 P+ k
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-58 P3 c' h m1 O% d
min, and cool in a stream of running water. Titrate this solution, using0 t( z0 V( @. \ ?: O9 G% F/ g* X
the standardized zinc sulfate solution as titrant, to the same fugitive
5 J3 _" r& u4 q0 F* o% u, b- Ryellow-brown or pink end-point as described above., @, I9 Y- F% c/ M
Calculation:) j" r* \3 k2 ^# X: j4 {& k
Calculate the percentage of aluminium oxide (Al2O3) in the sample
8 ~- P' k0 ~9 \taken by the formula:: n" ~; C9 z Q7 C# R: @
% Al2O3 = 100 × (0.005VT)/S
# U1 V- N: f2 m/ Xwhere
9 n: o4 p2 _) b9 S9 v2 PV is the number of ml of 0.01 N zinc sulfate consumed in
7 L3 s/ y5 N ]2 B" d0 R! c! ^" rthe second titration,0 v0 V4 ^: ?. _' o! q& ?/ ^$ }
T is the titre of the zinc sulfate solution,; @) O1 U9 L: T0 H( U( ?+ B, ~7 q
S is the mass (g) of the sample taken, and
" F3 F- ^ X& d0 l$ h0.005 = 500 ml / (1000mg/g × 100 ml).
8 I+ t( \) Z) ~! e" X/ b( ^Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica0 d) U/ b3 d9 n4 T" U/ r
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
4 s; x* i( @- QHeat gently over a Meeker burner, while swirling the flask, until. @/ H' i( t. o, r6 G
decomposition and fusion are complete and the melt is clear, except; r7 J4 W0 v) V/ @) \$ W9 Z
for the silica content, and then cool. (Caution: Do not overheat the! h s, e; |$ {2 `3 z% R
contents of the flask at the beginning, and heat cautiously during. H# ^# p9 R* g1 U! R
fusion to avoid spattering.)
) {; p1 u8 |3 q& T( B* z5 XTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat2 L4 `7 L( V; o$ s; W5 F- Q: @
carefully and slowly until the melt is dissolved. Cool, and carefully add* e7 p H6 R; V9 v, M$ S5 }
150 ml of water by pouring very small portions down the sides of the& `0 j8 w, c& ^2 d4 k0 `1 z
flask, with frequent swirling to avoid over-heating and spattering. Allow9 C' b8 X" p ]9 {- l" }
the contents of the flask to cool, and filter through fine ashless filter. l$ k# h8 `( U2 J4 K) N8 O# H
paper, using a 60 degree gravity funnel. Rinse out all the silica from
, k# @+ Q3 W) l3 v/ K W6 othe flask onto the filter paper with sulfuric acid solution (1 in 10).
0 Z4 L4 m2 z1 H- M/ mTransfer the filter paper and its contents into a platinum crucible, dry in6 ?) P( M p0 i, ?; j: u( }* u
an oven at 1200, and heat the partly covered crucible over a Bunsen
* p3 d( W4 c& ]) x: V* U1 U4 T9 Dburner. To prevent flaming of the filter paper, first heat the cover from
4 ^7 u {& |# H m. ?+ S) \$ |- @above, and then the crucible from below.6 ]* c) e( X7 O0 I8 g( _
When the filter paper is consumed, transfer the crucible to a muffle
0 z, T/ a6 I5 b$ w! ?- A4 Rfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and9 _; [. v: ~- F1 g
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
: G; p5 l$ p- J0 T- z. }hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
! z5 B% Z1 M3 T6 D" o' X) }+ Pon a low-heat hot plate (to remove the HF) and then over a Bunsen
/ x) e6 m2 E) J7 S2 {: }0 _burner (to remove the H2SO4). Take precautions to avoid spattering,. l( p7 l9 r* I' |
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
* ]( ^5 Z2 N/ |' \- U: C9 U* Z5 Udesiccator, and weigh again. Record the difference between the two
2 |$ c1 ]0 n9 D( Bweights as the content of SiO2 in the sample.8 m- r* J0 e a, M# u9 x0 I9 w
METHOD OF ASSAY
b5 z- a, U1 V uAccurately weigh about 150 mg of the sample, previously dried at 105o3 X; m) a7 j! ~, e2 Z2 a0 T: e) K2 q; R
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
1 P9 o; s2 v8 T* E0 a1 i7 wand shake until a homogeneous, milky suspension is obtained. Add 30
# E o' }, [: s# @ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
6 l' q5 ]* x2 x2 E! F6 Sheat gently, then heat strongly until a clear solution is obtained. Cool,
# ~( c" E" Z: D2 ^# I% {then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
# e. y' H; _4 w3 }: k( sacid, and stir. Add 3 g of aluminium metal, and immediately insert a
4 H ~* o, x5 M, q2 hrubber stopper fitted with a U-shaped glass tube while immersing the
4 ]! \) A! B( H. U+ v1 Z5 @other end of the U-tube into a saturated solution of sodium
* S& ?. s1 z+ u% B$ bbicarbonate contained in a 500-ml wide-mouth bottle, and generate
6 D6 A9 c6 ^' nhydrogen. Allow to stand for a few minutes after the aluminium metal/ L: M6 H6 A% n+ g
has dissolved completely to produce a transparent purple solution.
1 }3 Y- t. A8 t+ l( R7 P1 h# WCool to below 50o in running water, and remove the rubber stopper3 t3 V9 |$ C. U, R& u: \
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
' N( R9 `) ^) {/ Z0 D) X$ y, Zsolution as an indicator, and immediately titrate with 0.2 N ferric
) E+ b5 e) [# y- [/ a! ?) P* Cammonium sulfate until a faint brown colour that persists for 30) _8 ~- z+ s0 M* ^( V0 {3 N9 }( D
seconds is obtained. Perform a blank determination and make any
4 |; F. O8 h ^; w0 Hnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is/ D3 Q4 g( c5 ]4 |3 v* }" n6 N
equivalent to 7.990 mg of TiO2.
c& }% o. P4 p' H |
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