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二氧化钛(钛白粉)
二氧化钛(钛白粉)
8 {. R* j, v" {* N% f, F
6 r9 b6 z: A- _JECFA关于二氧化钛(钛白粉)的结论
- f7 y: P5 S, l8 W* L# G: T1 ^6 C/ c* D& z
摘要: 2006年JECFA关于二氧化钛的结论
- x/ G% ]+ H" nADI值:不作限制。$ q, W$ o4 M/ o
功能:着色剂
; \% x+ e N4 m( j& T. o% T- Y0 c/ z( X, O
TITANIUM DIOXIDE
: \( g( y3 b" R8 D+ A& r& XPrepared at the 67th JECFA (2006) and published in FAO JECFA& c D+ p( u- y/ v
Monographs 3 (2006), superseding specifications prepared at the 63rd
' u* f3 v9 y! A# U" C6 rJECFA (2004) and published in FNP 52 Add 12 (2004) and in the) `+ d& m" }& [( i; `& p1 [% U
Combined Compendium of Food Additive Specifications, FAO JECFA
9 `5 Y n) v2 K& IMonographs 1 (2005). An ADI “not limited” was established at the 13th
& ^! `* t: j+ j4 L3 MJECFA (1969).& o. G) o3 R: j
SYNONYMS
+ _/ L* O- D: w: v9 N0 r5 YTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
) l1 Q1 C; c4 r3 u; a2 g" |DEFINITION
, _! P4 x7 N' W9 V% c$ ZTitanium dioxide is produced by either the sulfate or the chloride' ?/ V' O& s1 }3 Z; ^+ g3 O
process. Processing conditions determine the form (anatase or rutile1 d& X$ |; G7 W6 p; l3 \
structure) of the final product.
$ Q. M3 C) X$ A( P$ ^In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
+ \: \' ~ |+ b& f. D8 J4 I9 jor ilmenite and titanium slag. After a series of purification steps, the" Q" n" t) w. c5 r' u7 W
isolated titanium dioxide is finally washed with water, calcined, and* t" {; I9 G, X& J
micronized.4 e% O r) ^' i' Q# [8 T
In the chloride process, chlorine gas is reacted with a titaniumcontaining
+ P' R1 Y. L! g# H! |mineral under reducing conditions to form anhydrous0 E; n! L _" x& @7 h
titanium tetrachloride, which is subsequently purified and converted to% V9 P4 K- g& Q; l9 g: `2 _3 h
titanium dioxide either by direct thermal oxidation or by reaction with y4 W3 h1 b8 S0 ?" N
steam in the vapour phase. Alternatively, concentrated hydrochloric
9 n# G! ?; L7 M' K3 C% b' uacid can be reacted with the titanium-containing mineral to form a4 D7 g0 W n+ g* E; t, P
solution of titanium tetrachloride, which is then further purified and7 M, z# i8 s! t, G) T. i' B' ?( ?
converted to titanium dioxide by hydrolysis. The titanium dioxide is9 M3 v& h/ Y- `& J2 M9 Z
filtered, washed, and calcined.
6 Z# |( S/ a# ^4 R* oCommercial titanium dioxide may be coated with small amounts of
& A& O; U+ p+ z2 F. Zalumina and/or silica to improve the technological properties of the
' \( D! R0 l! iproduct.
* x4 r7 Z6 l9 o7 `C.A.S. number 13463-67-7
' t3 N: a4 _) d1 X9 cChemical formula TiO2
3 w+ _: C+ y, ?0 ]/ s5 o1 [Formula weight" Q8 ^; v6 ^! F* p! h* e
79.88
# k2 a! R/ z+ H$ t% H7 rAssay. L8 G/ I; \1 A+ ?
Not less than 99.0% on the dried basis (on an aluminium oxide and4 t* X9 Q$ k4 C; S$ N
silicon dioxide-free basis): N$ x; \3 D$ V- k$ f' C4 f. d
DESCRIPTION
, `( l6 c$ {) r& |; J& jWhite to slightly coloured powder
2 x: K. ]' U, ~FUNCTIONAL USES
[3 [$ H9 j5 jColour
: b6 z8 L9 |/ o1 \$ T" ~CHARACTERISTICS0 u: T" X2 ~3 Y7 O1 B# O
IDENTIFICATION
. V" x0 Q6 m& B V: Z7 b+ E9 NSolubility (Vol. 4)
, s! F: _, x- I$ a( Y6 k! Y/ VInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
, E( y+ `+ Y% f% {- r C0 j! {solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
( j* m h- n" y8 w9 {% osulfuric acid.+ ?" m, y5 u: N( \! K* w
Colour reaction
9 K3 x9 ^7 H- O& M' x4 @1 a- BAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of6 k& v; K! w' w& C8 U1 X
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
" G4 X* @# w; x& t4 Kwater and filter. To 5 ml of this clear filtrate, add a few drops of9 H$ q& ?4 E/ K
hydrogen peroxide; an orange-red colour appears immediately.5 B) X5 x/ A( Z S
PURITY8 t. y+ y8 _7 u% \
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)8 p1 c6 h9 R9 P# d
Loss on ignition (Vol. 4)
+ `# h' d( P0 n3 s3 A- q/ iNot more than 1.0% (800o) on the dried basis' m, f! G/ a7 l
Aluminium oxide and/or; W; F" X& S( j7 ~+ w
silicon dioxide5 O% Q9 @, ]: f! p9 j
Not more than 2%, either singly or combined% n7 L7 N* Y! a+ q/ z: f( v
See descriptions under TESTS) U( B* h- ~; b/ i5 A2 j
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing9 |0 }: F2 j3 K: J( T6 c3 B
alumina or silica.
. a: n( {& T* x; g+ [4 D$ H8 MSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
' |' Y$ K" V+ pplace on a steam bath for 30 min with occasional stirring. Filter
8 K" A7 z8 B/ b" D Wthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
! h/ h4 f0 a. n- C) vwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the& D- H% x* o2 D: \3 X* u
combined filtrate and washings to dryness, and ignite at a dull red
4 |; a R( n9 yheat to constant weight.
( h- u" D, N. A0 @( kWater-soluble matter
6 g: h$ g+ h6 @( _; p) m$ w$ v(Vol. 4)9 k w) ^' C4 J/ M8 f4 ^
Not more than 0.5%
: X# H2 u0 b: TProceed as directed under acid-soluble substances (above), using
8 D& l( g, j. dwater in place of 0.5 N hydrochloric acid.% M0 _( z$ {: E# r
Impurities soluble in 0.5 N5 ~" t7 |2 R1 z: x8 A
hydrochloric acid
' Y3 W0 t( h2 b/ v6 E- MAntimony Not more than 2 mg/kg B8 I& g; i8 ~) _# w& w
See description under TESTS
) V8 t3 I$ ~+ cArsenic Not more than 1 mg/kg
9 e' B% z/ n: ]- PSee description under TESTS
, a; G, ^8 c. I4 A! O7 P+ N% aCadmium Not more than 1 mg/kg* m. a2 @1 n2 n1 D5 Y( M5 Y2 L+ y
See description under TESTS
, j" A' [2 }) h! z* c) \Lead: o. w3 u: z) y6 P$ j! j4 C1 g+ }
Not more than 10 mg/kg7 Y! _( R/ X1 O6 {4 s& ~
See description under TESTS4 e9 Z. m4 Z4 Q% A+ g; `
Mercury (Vol. 4) Not more than 1 mg/kg
5 s) [, y2 ?9 A5 I; {( N1 WDetermine using the cold vapour atomic absorption technique. Select a3 ?+ P5 A* Z/ O% S/ |1 m ?4 E
sample size appropriate to the specified level
0 Q4 T6 Q% ~, {& n. @TESTS
4 h5 A1 p5 m8 `& J/ h5 uPURITY TESTS8 ~1 e' T1 l% q$ B8 ?# E" y- {! s: }1 R
Impurities soluble in 0.5 N
! l+ K4 m3 Z9 s9 ihydrochloric acid
: V8 }; y( m$ ]Antimony, arsenic,
. f- X' h8 e" z5 h5 acadmium and lead6 c% i$ U `+ L
(Vol.4)6 H5 u# T. n- @+ M' |
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
; b% I& A+ C# f* c: [- c+ s; T2 [hydrochloric acid, cover with a watch glass, and heat to boiling on a
1 Y. n& ]# V1 k4 F' fhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
8 L4 d3 {3 Q8 q* Y/ Ocentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved% `" ]. i$ ]9 X% _9 ?/ f3 o& L& {* V
material settles. Decant the supernatant extract through a Whatman
* B* ?) r$ n3 z6 g& A5 O: DNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
: v& q5 k& L5 ^7 tvolumetric flask and retaining as much as possible of the undissolved5 g/ ~/ J' M- l- F5 f0 r
material in the centrifuge bottle. Add 10 ml of hot water to the original7 F5 Y* U" v3 x$ S3 j8 G. C# J
beaker, washing off the watch glass with the water, and pour the! l* V. v9 H9 {) K$ e
contents into the centrifuge bottle. Form a slurry, using a glass stirring8 a ~8 ~- x8 V. j5 |8 \
rod, and centrifuge. Decant through the same filter paper, and collect
: J' g7 a- J1 d9 y" m2 ~+ g5 r0 othe washings in the volumetric flask containing the initial extract.) I' H; V3 C6 J6 Q1 G
Repeat the entire washing process two more times. Finally, wash the/ g& g/ ^; {9 {/ J: a( |
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask2 V H5 ]3 r7 v" c+ E. M- J- V
to room temperature, dilute to volume with water, and mix.
& z7 x5 S6 w* C6 W3 j, Q6 `# }Determine antimony, cadmium, and lead using an AAS/ICP-AES; N* p# p0 s7 l1 q
technique appropriate to the specified level. Determine arsenic using the
* t0 _% n" ?# f5 t+ [/ [/ G+ IICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
2 v) R' N9 h; F6 AMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than1 l* u" |3 M r: O G
1 g. The selection of sample size and method of sample preparation% {4 {1 I+ a" U, b
may be based on the principles of the methods described in Volume 4.$ y% Y; X/ @- X* n4 b& Q* b' N
Aluminium oxide Reagents and sample solutions
: f$ C' g3 K8 r" ]4 L0.01 N Zinc Sulfate5 K, O* l- S& P: a% ^* O
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to `1 ?- B6 ?- q) m
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
/ v V5 K) ?3 e; E @of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
; B+ X% j& `" e4 U3 Kconcentrated hydrochloric acid, heating gently to effect solution, then
. Q1 u( p. W% ?transfer the solution into a 1000-ml volumetric flask, dilute to volume
+ g3 T; _' Y0 n+ `with water, and mix. Transfer a 10 ml aliquot of this solution into a 500$ x: [7 Q! M: G% |1 ?% u2 t
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
+ ^% U1 M1 p1 o& _concentrated hydrochloric acid, add 1 drop of methyl orange TS and
9 l# o8 K' ?) {" q! K25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
8 x/ M% J- k* T0 Y. j' kdropwise, ammonia solution (1 in 5) until the colour is just completely" N( z4 {) Q% u! y/ c+ [
changed from red to orange-yellow. Then, add:$ H% X8 z2 z/ n" F3 {9 j! f
(a): 10 ml of ammonium acetate buffer solution (77 g of8 A: x2 K# \. P4 x9 d7 b. v/ H
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
2 V3 F, ?5 P. l) Z2 e1000 ml with water) and' W5 u; ~- ?( H+ m+ ]( }
(b): 10 ml of diammonium hydrogen phosphate solution (150 g) F# Q, U6 n9 s8 l6 S
of diammonium hydrogen phosphate in 700 ml of water,
( r7 `* y6 I: padjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,: j! n) k; r& _* }9 H
then dilute to 1000 ml with water).
4 t4 G0 _+ z( x! |. C! D% t& c S9 N4 MBoil the solution for 5 min, cool it quickly to room temperature in a
' X. l( y3 {0 h; Y, V+ s. Q. Kstream of running water, add 3 drops of xylenol orange TS, and mix.# [. l; g- i; R
Using the zinc sulfate solution as titrant, titrate the solution to the first
5 ~& @( C' ], t9 q# eyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
. m/ g1 V6 h4 SThis titration should be performed quickly near the end-point by
* q7 b, e4 J/ X6 w. P5 Fadding rapidly 0.2 ml increments of the titrant until the first colour, x4 e% F$ N" ?0 S) @* V/ J. O. k
change occurs; although the colour will fade in 5-10 sec, it is the true4 {. |: S6 @( J* v4 j
end-point. Failure to observe the first colour change will result in an
$ l. G, F* r0 { kincorrect titration. The fading end-point does not occur at the second% e2 T' H% }6 J9 t, ?
end-point.)
/ y( {( a' D5 |" [/ sAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a" j1 C: `, B% y7 X: ]# X& u4 _4 C4 W
stream of running water. Titrate this solution, using the zinc sulfate
$ }2 P' }0 U. n4 l/ n3 zsolution as titrant, to the same fugitive yellow-brown or pink end-point
* l( K2 Y: D9 b+ _' las described above.2 w* p" C [$ S6 c$ @8 ?
Calculate the titre T of zinc sulfate solution by the formula:
) S" i) w& T2 j- l; {% s) J, BT = 18.896 W / V
( V. W" q o( Q' a4 A5 Cwhere5 B2 o0 C2 X( y
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
2 }# K/ i* q; G! O8 h$ H: `' Z# pW is the mass (g) of aluminium wire
; @0 q9 q- D: _" T$ zV is the ml of the zinc sulfate solution consumed in the
$ t" u3 E) _4 t2 Vsecond titration
" n/ e) w1 z& i( Y" M1 O0 j18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and0 q0 k/ p) }5 T% G9 `7 y
R is the ratio of the formula weight of aluminium oxide to+ H# t; l4 o% b6 n
that of elemental aluminium.- Q3 w6 @4 o4 p5 ]1 T, j7 ]% u# Q
Sample Solution A/ M3 G( v5 {, d0 A# f7 N: C' _
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
3 J8 n& ^; W; C! ~( p E xglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
) E8 G& J9 b) _8 X( H(Note: Do not use more sodium bisulfate than specified, as an excess" Q, x% M. ]' W% q
concentration of salt will interfere with the EDTA titration later on in the
4 Z& f( u3 r9 H) _* {6 R+ eprocedure.) Begin heating the flask at low heat on a hot plate, and
1 {( o& D/ ~6 i( P+ {- @& B# Bthen gradually raise the temperature until full heat is reached.
0 P& x8 g/ |+ j+ j# ^9 ]3 H& J(Caution: perform this procedure in a well ventilated area. ) When+ o& F- c+ r. m: j1 H' b6 J5 o# Z
spattering has stopped and light fumes of SO3 appear, heat in the full6 B- h7 W u7 `) B ~% P' [7 a
flame of a Meeker burner, with the flask tilted so that the fusion of the
* A( Z( Q+ m" p, Y+ Y4 Ssample and sodium bisulfate is concentrated at one end of the flask.# p5 |- X5 B' Z2 `/ {! Q& r6 x) D
Swirl constantly until the melt is clear (except for silica content), but4 y# z! y {, W$ K
guard against prolonged heating to avoid precipitation of titanium
" k `/ u; {. e9 D6 {0 ?dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until E2 a6 k# ?9 d; m5 H
the mass has dissolved and a clear solution results. Cool, and dilute to4 M5 }/ [% M& ~ A b0 w X
120 ml with water. Introduce a magnetic stir bar into the flask.
) l+ L6 Z- C' u# i" K# c% KSample Solution B k+ I% ~( R) b9 F9 a5 S( Q( s9 h) D
Prepare 200 ml of an approximately 6.25 M solution of sodium
/ p; N0 Y7 C3 G' [$ j& P; w3 _hydroxide. Add 65 ml of this solution to Sample Solution A, while. V, E" m- P: {4 h2 v; V. M) {. U& c
stirring with the magnetic stirrer; pour the remaining 135 ml of the
" M( c- s: g8 J" salkali solution into a 500-ml volumetric flask.( o f. F. L2 p: H% ?) N" C
Slowly, with constant stirring, add the sample mixture to the alkali% J( B( h, g! [5 W4 F" b" ?9 m4 o
solution in the 500-ml volumetric flask; dilute to volume with water,
; U) M2 k3 y4 U9 dand mix. (Note: If the procedure is delayed at this point for more than
9 @6 F2 F% R0 _- m, v2 hours, store the contents of the volumetric flask in a polyethylene) |7 k- V$ e) y: Z& o, | l
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),* F1 v+ v$ K$ T( k
then filter the supernatant liquid through a very fine filter paper. Label4 N8 L* c5 W; g- q! y
the filtrate Sample Solution B.7 H2 ^9 n) @9 F8 C, Q" A
Sample Solution C
! t2 |* U4 g) C$ p7 z# nTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer( y0 r9 M% {. ~8 z2 ]
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid; D$ i, a8 \- [" J2 m
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
7 X) G3 t0 W; q5 N+ I7 W+ nM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
5 N: `- @7 ^" V! r$ ? mknown, calculate the optimum volume of EDTA solution to be added
/ b% b* x) \+ @2 Gby the formula: (4 x % Al2O3) + 5.]
* p! ?9 X1 J; }. G1 q. ~- EAdd, dropwise, ammonia solution (1 in 5) until the colour is just
/ ]8 L5 C5 m5 [completely changed from red to orange-yellow. Then add10 ml each
H3 y+ Z* G/ M9 v- Y a7 k* lof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to- h$ t b. g% U6 q$ ]. q6 z0 _
room temperature in a stream of running water, add 3 drops of xylenol) C9 A# _, G' ^, w
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
, O) B; F6 N" p- Kbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
7 j" n" u/ d% Q3 f `. |pH, a pink colour indicates that not enough of the EDTA solution has
! s& U$ k( u) e7 {0 k' @been added, in which case, discard the solution and repeat this
5 W6 W6 |2 { J* R$ tprocedure with another 100 ml of Sample Solution B, using 50 ml, A. w% {. ^$ ? ^; J& j
rather than 25 ml, of 0.02 M disodium EDTA.
( l2 ?9 W; C# \Procedure' S7 Q! I4 [: y) s
Using the standardized zinc sulfate solution as titrant, titrate Sample
% K/ j9 [( S7 K2 U( N- {Solution C to the first yellow-brown or pink end-point that persists for, G( S$ `7 y0 ^, m& u4 r( A0 v. l
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
- w2 ]% ?5 u) ^$ htitration should require more than 8 ml of titrant, but for more accurate4 X% V9 N* d; z7 o! W
work a titration of 10-15 ml is desirable.
# v+ z' v' a- i* P8 e {) eAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
V( Q+ _, |1 e. jmin, and cool in a stream of running water. Titrate this solution, using
C- W8 i$ L4 N$ Vthe standardized zinc sulfate solution as titrant, to the same fugitive5 s, }; m R( A
yellow-brown or pink end-point as described above.& I+ \3 Q+ _% v( |: O8 P
Calculation:& j- o4 R$ d* ]: t
Calculate the percentage of aluminium oxide (Al2O3) in the sample/ L0 B" X( I, n0 N g9 ^; O# a: f
taken by the formula:
5 S }+ z1 A! k! I! o0 F% Al2O3 = 100 × (0.005VT)/S
8 z( K! e& n: z' L! Rwhere8 z, Y9 f/ V9 z+ H1 ~2 u% }" o+ c
V is the number of ml of 0.01 N zinc sulfate consumed in; q/ v( Y' @3 H* ^0 m" H6 w6 n9 b
the second titration,
7 s- L! I( o) Y9 x7 {4 @* M8 ST is the titre of the zinc sulfate solution,# W- |" T3 w A m5 M" k! r
S is the mass (g) of the sample taken, and% X0 J6 K6 \# x5 e% a
0.005 = 500 ml / (1000mg/g × 100 ml).+ ^- \/ E6 @8 G; W% b
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
# ]/ K' [; b! Uglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
: [; S* ]. ?! p2 c+ ]7 g( sHeat gently over a Meeker burner, while swirling the flask, until
% f; X: C# z& v- \# {& N: tdecomposition and fusion are complete and the melt is clear, except" ^: [* p0 ^. Y9 \. ]
for the silica content, and then cool. (Caution: Do not overheat the
, C& ]8 g2 s# K3 P' d0 h; dcontents of the flask at the beginning, and heat cautiously during
5 e+ V% _; h( F! [) ?7 N; afusion to avoid spattering.); P/ o, [5 G; O5 h, i) [
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
. p- n+ q/ z% j Z- j) N* ~carefully and slowly until the melt is dissolved. Cool, and carefully add
( U! Z$ d4 J( L& a) Q150 ml of water by pouring very small portions down the sides of the
4 o. m# q' S6 fflask, with frequent swirling to avoid over-heating and spattering. Allow
8 b" W0 R. C: l* c O c9 d( Cthe contents of the flask to cool, and filter through fine ashless filter( H9 H6 l7 {+ R) C
paper, using a 60 degree gravity funnel. Rinse out all the silica from
+ ~+ E3 m. \: a) Athe flask onto the filter paper with sulfuric acid solution (1 in 10).
. Z8 q2 m$ p; m2 [4 aTransfer the filter paper and its contents into a platinum crucible, dry in
: y) b X# M1 E$ fan oven at 1200, and heat the partly covered crucible over a Bunsen
% v2 w) f% ~+ K# }$ l2 t) l9 ?8 }& Kburner. To prevent flaming of the filter paper, first heat the cover from1 F; } z3 i0 y5 u
above, and then the crucible from below.
1 i# |+ H5 C" G; j6 F# M' z, d% \When the filter paper is consumed, transfer the crucible to a muffle" A7 a3 d/ f- ]2 K- i8 x
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
% V* o/ Z/ ~. m% N( ~weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated. V" [( S# |4 X
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
4 y* B- i& ^7 u0 v4 H" a7 K+ I* w% aon a low-heat hot plate (to remove the HF) and then over a Bunsen6 s, ]) G- o [& [
burner (to remove the H2SO4). Take precautions to avoid spattering,9 t Z+ ^9 A" N5 m+ Z# e9 w; m
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
% m. u) k8 J( y; G* Kdesiccator, and weigh again. Record the difference between the two
3 `) W# n" i& `4 N0 qweights as the content of SiO2 in the sample.
# Y2 f; q% a* ?METHOD OF ASSAY5 O2 T- [0 P% L' v3 M5 o P
Accurately weigh about 150 mg of the sample, previously dried at 105o7 G5 T9 F+ v5 A5 _) X
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
! d8 W# R9 \4 Vand shake until a homogeneous, milky suspension is obtained. Add 305 X' D: F- Y$ _, a. P; I8 L7 C
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially' }+ f% I# T4 A. |% o3 i
heat gently, then heat strongly until a clear solution is obtained. Cool,' [* k# K. W ^, S4 G* X1 L$ }
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric3 q; I+ y% A x& e" d
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
/ X4 u! |& i. Z; vrubber stopper fitted with a U-shaped glass tube while immersing the
. ]+ C9 D: G2 y1 v1 f5 G% c. Gother end of the U-tube into a saturated solution of sodium
& q6 y* m9 O" }" hbicarbonate contained in a 500-ml wide-mouth bottle, and generate$ ]4 W7 C$ Y8 O9 [! y
hydrogen. Allow to stand for a few minutes after the aluminium metal; @) ~4 V1 C! F1 p8 P* z% S+ C
has dissolved completely to produce a transparent purple solution.: {7 K @3 M, y( o: q
Cool to below 50o in running water, and remove the rubber stopper
8 ^, F+ E5 L! f5 m: ~# o4 }carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
6 l- d- q* g8 @% ?$ f) N( b( dsolution as an indicator, and immediately titrate with 0.2 N ferric& W' ^! \7 v3 i0 X/ U( @
ammonium sulfate until a faint brown colour that persists for 30, l: C/ X- Y- L3 h; ~4 G% c
seconds is obtained. Perform a blank determination and make any K; L4 z/ v; |1 w
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
1 s+ f( {1 G: v! D \ E( J8 Aequivalent to 7.990 mg of TiO2.
! r8 o( J" m3 K7 R+ D |
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