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二氧化钛(钛白粉)
二氧化钛(钛白粉)
( d/ c2 x; [' u" Y4 {% C0 x$ z& h
% ~% T, _5 h j4 M; Y5 W2 }+ B; dJECFA关于二氧化钛(钛白粉)的结论( E! x0 y* L$ m. e; d8 I7 F4 W# F: ~
9 w! D+ B/ M6 @+ H摘要: 2006年JECFA关于二氧化钛的结论
: O3 ^! ? m$ F2 J3 _* G& JADI值:不作限制。% f# O3 p. b& [( `7 }6 v/ @
功能:着色剂
5 v0 Q. @7 A& R5 J, o5 X
6 R# w( U+ ^, `7 _* W9 ^" ^TITANIUM DIOXIDE9 \9 A }% L5 s! H# u
Prepared at the 67th JECFA (2006) and published in FAO JECFA; r4 l, W" C) ]$ q
Monographs 3 (2006), superseding specifications prepared at the 63rd
3 I9 o# g& O& D6 d$ H* MJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
; j3 E+ y! l( G2 [. V" {Combined Compendium of Food Additive Specifications, FAO JECFA8 M% T( X9 V W4 z: M$ n
Monographs 1 (2005). An ADI “not limited” was established at the 13th/ r2 ~4 S; i4 V- T3 E9 m
JECFA (1969).+ X+ \' D* T' V1 @3 \2 m
SYNONYMS1 Z W6 ^% ]) I. z+ l
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171; H7 a- c. m) }9 b6 l
DEFINITION
: j4 {# C) R) l7 e( F! mTitanium dioxide is produced by either the sulfate or the chloride
! C `8 |7 S7 ^6 X7 }3 sprocess. Processing conditions determine the form (anatase or rutile# g" K5 c2 Z( I( R7 x# E
structure) of the final product.2 J$ h( E( o( X. P5 W2 c
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
8 L4 g2 b; S4 t) @& z: V4 ior ilmenite and titanium slag. After a series of purification steps, the
9 h% v( j$ y5 _/ ?4 I |isolated titanium dioxide is finally washed with water, calcined, and$ p+ c# r% y' h8 D$ V" @; F
micronized. O( \6 q( _, z; f) D, W; [
In the chloride process, chlorine gas is reacted with a titaniumcontaining' P' |) e9 c9 I+ u1 J8 D4 Q
mineral under reducing conditions to form anhydrous2 `( A! ^. P6 H2 Q$ Y
titanium tetrachloride, which is subsequently purified and converted to
# d7 g, I; x* I7 Wtitanium dioxide either by direct thermal oxidation or by reaction with6 N' \" t/ _6 b: {" t) l
steam in the vapour phase. Alternatively, concentrated hydrochloric5 `' S. `% x; U- Y: h
acid can be reacted with the titanium-containing mineral to form a- Z- H& v n8 f& F- V3 Q% I/ u. s f
solution of titanium tetrachloride, which is then further purified and3 C( w$ y1 C1 p$ M1 ?, T) X$ {& p
converted to titanium dioxide by hydrolysis. The titanium dioxide is
4 w" \3 I! f, U' s$ q8 a# [filtered, washed, and calcined.
4 n4 S- [+ y4 W: E' }- jCommercial titanium dioxide may be coated with small amounts of
1 I7 |4 Q, @% ~5 P* ralumina and/or silica to improve the technological properties of the
2 A# y n7 M) qproduct.$ z# q# _" u$ Y7 P9 b. J
C.A.S. number 13463-67-7
/ n6 q* y* t, v, [" T IChemical formula TiO2
; X U. x9 H {0 M8 {Formula weight
0 e+ |: f0 ^/ @% k9 r7 P# ?79.88
: e8 q8 S; [; T8 P9 k! lAssay+ X- A: o3 _; D4 I: |) }
Not less than 99.0% on the dried basis (on an aluminium oxide and1 p2 p& l1 _# r3 i C
silicon dioxide-free basis)9 @5 r3 O, S3 d2 v
DESCRIPTION4 S7 c. r0 T4 ] w/ O
White to slightly coloured powder6 \2 G1 K$ J Y+ J2 w
FUNCTIONAL USES
" I, l$ M$ v# uColour3 N0 r4 W0 k% v0 A7 D; K
CHARACTERISTICS
9 P2 t: s" q- k- SIDENTIFICATION
: K6 z8 n3 Y' q$ K. DSolubility (Vol. 4): b9 E, n' s0 d
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
2 Q% u$ r0 ]2 X+ ^% A( ?solvents. Dissolves slowly in hydrofluoric acid and hot concentrated* h7 O$ Y, \6 I% E4 m) _
sulfuric acid.
% ~4 L* k A# C6 Z; [0 n5 f% b$ w) vColour reaction- M( L$ M+ i0 I) ?
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
9 k& t3 S, r" L" ?0 A8 Lsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with, {' K( l, n1 U! ?& r
water and filter. To 5 ml of this clear filtrate, add a few drops of, C9 {6 P# {- l. p+ j
hydrogen peroxide; an orange-red colour appears immediately. i' ]% }7 v. X9 o5 e
PURITY
. w1 c2 c. H: q* @ e; VLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)4 B6 ^; ~7 O4 s
Loss on ignition (Vol. 4)( o @1 b5 l4 I/ D! k6 `
Not more than 1.0% (800o) on the dried basis2 P0 w& G& F: w; A) y) Y
Aluminium oxide and/or& M; o! H; _% J3 ~/ Q& v
silicon dioxide1 ?8 ], O* c% ^0 V% _1 l
Not more than 2%, either singly or combined" H/ ~4 y% R& \
See descriptions under TESTS
9 z% ^! P( ^( ?Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing0 {, I: z+ z0 ?: j
alumina or silica.
2 o, X$ h! {& WSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
9 f9 o( d% [% n+ Y/ n& kplace on a steam bath for 30 min with occasional stirring. Filter9 p1 n, ?3 l) Z" |2 [
through a Gooch crucible fitted with a glass fibre filter paper. Wash
/ I, v. g8 V( t# w2 hwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the2 J3 k' |2 d5 L- h2 \/ y
combined filtrate and washings to dryness, and ignite at a dull red
' z' t+ c( K/ U( }: Dheat to constant weight.
; q! G) U% N; n, {Water-soluble matter
}: f0 X( ^! A(Vol. 4)
+ m* B9 v+ C! g" P4 x* CNot more than 0.5%
5 Q6 q( q* {# e% L; v# hProceed as directed under acid-soluble substances (above), using" l' l5 ^* {" P @6 N* P
water in place of 0.5 N hydrochloric acid." c$ C2 D( f+ p$ D7 ]
Impurities soluble in 0.5 N
) V: }( \ q( [4 e. s( W" S+ }hydrochloric acid
+ ~9 P6 r& A* C- u4 M& ^( F1 z Z, }Antimony Not more than 2 mg/kg2 i; a& t& R* R
See description under TESTS! i& w4 I( U% ?$ T( ~: A
Arsenic Not more than 1 mg/kg; y5 w8 `8 J0 S, j: v! D
See description under TESTS5 V6 X7 g$ K! n! `; W# Z7 w U+ E
Cadmium Not more than 1 mg/kg5 _3 s+ O1 A4 W, c
See description under TESTS8 [0 g) q! V, x/ ^/ J8 h' a+ I9 S
Lead+ }) P. X6 t3 ]/ S
Not more than 10 mg/kg+ e+ x9 ? d4 c+ t
See description under TESTS! f; a! ]8 l ]$ z& } R
Mercury (Vol. 4) Not more than 1 mg/kg, R! ~6 D5 Y6 ^5 V
Determine using the cold vapour atomic absorption technique. Select a: }4 u6 D# K3 D' s5 B) R
sample size appropriate to the specified level
) @' j) v/ `! w/ E: V: OTESTS
% P% E, i) V; L5 |$ ePURITY TESTS
; d' N% ?; n" M; h& j/ z( {Impurities soluble in 0.5 N
/ I, W9 f; O) n8 }# Uhydrochloric acid
( v( m5 W/ J' y! s3 qAntimony, arsenic,
c6 `. c& c5 M4 {* I6 J! xcadmium and lead6 `3 m7 T7 D, N7 ~( T' ?1 R
(Vol.4)' z) v9 z2 j& @
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N$ H/ I0 g4 Z3 ]0 _: |5 D
hydrochloric acid, cover with a watch glass, and heat to boiling on a
4 L, |2 x: E0 u) d& |2 p2 s! mhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml' {' ?* C- E. y |8 t+ ?! W- _
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved0 \+ ~9 x8 D( r1 C! H
material settles. Decant the supernatant extract through a Whatman. o; Z" a4 g$ \3 m5 V
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
$ ]7 [1 r0 C' z: ovolumetric flask and retaining as much as possible of the undissolved
% Y# @( g7 ` R3 a5 |8 k4 dmaterial in the centrifuge bottle. Add 10 ml of hot water to the original5 b( J+ O4 w' n8 A# E
beaker, washing off the watch glass with the water, and pour the
3 E6 M w+ @6 K$ Ycontents into the centrifuge bottle. Form a slurry, using a glass stirring2 M; z/ }9 o- a# C2 C! x. h
rod, and centrifuge. Decant through the same filter paper, and collect
) Z3 v) }0 F/ R4 cthe washings in the volumetric flask containing the initial extract.
* j" E1 B# f$ L! R% QRepeat the entire washing process two more times. Finally, wash the
; l8 V: x% I. O$ c" A4 r ifilter paper with 10 to 15 ml of hot water. Cool the contents of the flask9 }3 [9 A7 [) C! z* p0 z
to room temperature, dilute to volume with water, and mix./ k; y) I0 u7 A) H' n1 s* l
Determine antimony, cadmium, and lead using an AAS/ICP-AES8 z) [, b! V3 j5 y4 M% n# r
technique appropriate to the specified level. Determine arsenic using the
% g/ x7 G: y) N" AICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
. W1 b8 D3 o( M* Y! ~' DMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than( U" O0 ?- @* p% I) r: `" N
1 g. The selection of sample size and method of sample preparation
, x1 H. q* a& r8 \: b2 omay be based on the principles of the methods described in Volume 4.
# ?! x, k) h3 y7 m8 bAluminium oxide Reagents and sample solutions( w8 h# N9 G4 I! M1 K2 N- a
0.01 N Zinc Sulfate
+ [0 p3 }* N, _7 ]' x0 r7 eDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
2 ^& L* _+ H3 H# Y, s& smake 1000 ml. Standardize the solution as follows: Dissolve 500 mg6 }/ e' x1 c. g" J; ]4 B8 q3 K
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
2 }9 |1 t l6 K* q) @4 Iconcentrated hydrochloric acid, heating gently to effect solution, then' g U9 O3 O$ m3 M% i. b9 k: R8 a' }
transfer the solution into a 1000-ml volumetric flask, dilute to volume6 C9 Y9 U& V& l1 y6 G5 ?* f7 Y. d7 v5 U
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
# o! |0 U$ Y3 a- Z& N3 z7 yml Erlenmeyer flask containing 90 ml of water and 3 ml of- k- C8 s. f3 P' {) h- x$ _2 u
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
' y0 b" R' d2 c1 F* e2 _25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,. P8 N5 z) T) l
dropwise, ammonia solution (1 in 5) until the colour is just completely
% ?. q: z) K- g X) echanged from red to orange-yellow. Then, add:+ `6 B2 q! {) B0 g
(a): 10 ml of ammonium acetate buffer solution (77 g of! E) T3 ~. |8 ]
ammonium acetate plus 10 ml of glacial acetic acid, dilute to2 F" z6 B% W0 M, z9 ^- |% m
1000 ml with water) and' B4 u! N( E, B A/ h; w
(b): 10 ml of diammonium hydrogen phosphate solution (150 g) _4 N+ i9 w1 e. v; u8 w
of diammonium hydrogen phosphate in 700 ml of water, ?% |: A N- b6 o0 {$ |( Y
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,/ V8 k8 x* }2 I( U3 j2 [+ a5 k9 t
then dilute to 1000 ml with water).
, u& q6 U4 ^3 OBoil the solution for 5 min, cool it quickly to room temperature in a! D) ~9 ?' W9 a/ f; {, z
stream of running water, add 3 drops of xylenol orange TS, and mix.9 Q( ]: R, w; Y( H r" f
Using the zinc sulfate solution as titrant, titrate the solution to the first* `8 o1 H' |) {- C6 C( T' s- c
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
8 J' J% C9 p- fThis titration should be performed quickly near the end-point by
5 P2 T. U7 Y! m& vadding rapidly 0.2 ml increments of the titrant until the first colour
7 |- k7 ]0 F9 k- I# }, vchange occurs; although the colour will fade in 5-10 sec, it is the true5 S) \" x$ X( X4 _+ o8 e
end-point. Failure to observe the first colour change will result in an
% C% ^- W: Y' q* j8 _; {incorrect titration. The fading end-point does not occur at the second& c: K* F/ o3 f' |: j
end-point.)* i: g% W: s) C, k, D
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a1 f5 b+ L8 X. r8 D# ^
stream of running water. Titrate this solution, using the zinc sulfate
) L( g5 Y+ x" psolution as titrant, to the same fugitive yellow-brown or pink end-point, [8 T: K$ a1 |: I/ u! O
as described above.
! i" z$ O0 D7 h$ F; jCalculate the titre T of zinc sulfate solution by the formula:
. C/ o X& e' o" D1 l4 @7 K( KT = 18.896 W / V: H0 c. O& ~, s7 I4 ?* i
where6 `- r2 c/ s8 h C" m+ A$ c
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution# o$ L7 h" c& Q: t
W is the mass (g) of aluminium wire
1 R2 b3 m# L, D: e4 u* LV is the ml of the zinc sulfate solution consumed in the
0 x% X. C& U" X# Wsecond titration' g" E, [1 J1 B+ e( w
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and- O% _6 {" \, M! j0 c) q1 W$ ~% ^3 U
R is the ratio of the formula weight of aluminium oxide to. P. y+ W+ L8 P4 c1 p
that of elemental aluminium.- ]6 l) b7 l+ I' \7 z; v
Sample Solution A
k. h7 g9 Z6 c. q {Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica9 j2 s/ @& A$ t% D$ K
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
/ E8 d, Z8 i, G8 [* P(Note: Do not use more sodium bisulfate than specified, as an excess
; u" ^4 }# O, Z" ~: Q5 Q3 Wconcentration of salt will interfere with the EDTA titration later on in the
, t. {" L6 j7 |3 \# F+ Nprocedure.) Begin heating the flask at low heat on a hot plate, and
4 t6 }4 K) |& Q Z0 e" Q6 U tthen gradually raise the temperature until full heat is reached." v1 y( ^% }0 B! q) s. A
(Caution: perform this procedure in a well ventilated area. ) When+ B+ @; d+ Q* H
spattering has stopped and light fumes of SO3 appear, heat in the full
* K2 j3 I h% ]flame of a Meeker burner, with the flask tilted so that the fusion of the2 J) x4 I% }! v! i% G+ @: l1 \
sample and sodium bisulfate is concentrated at one end of the flask.
2 q B& H0 o" j% D- D( ?Swirl constantly until the melt is clear (except for silica content), but
0 c6 Z- a" w6 `# wguard against prolonged heating to avoid precipitation of titanium
" t- w* g4 W& d: Bdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
, Q e7 b7 B# ]' sthe mass has dissolved and a clear solution results. Cool, and dilute to Z$ K; i8 _% T" I) s' b) s A! ^
120 ml with water. Introduce a magnetic stir bar into the flask.% I( g- F' ^7 D% P
Sample Solution B
) O5 A5 K9 C) g3 p; |8 e" i s7 PPrepare 200 ml of an approximately 6.25 M solution of sodium
V5 s4 V' h4 A0 r& |hydroxide. Add 65 ml of this solution to Sample Solution A, while
& b; @7 V) {' o1 R1 j7 Nstirring with the magnetic stirrer; pour the remaining 135 ml of the' [, Z( I( S0 y6 R) U4 V% f* `
alkali solution into a 500-ml volumetric flask.
% Z, }. K( C% g/ {# fSlowly, with constant stirring, add the sample mixture to the alkali, v# l2 v4 z- x9 i6 B
solution in the 500-ml volumetric flask; dilute to volume with water,
4 E5 n" x, H% band mix. (Note: If the procedure is delayed at this point for more than
+ I" { _$ Z% d2 hours, store the contents of the volumetric flask in a polyethylene
( Q) I$ ^- P9 s' [% Nbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),* N. N7 b% H% h" r
then filter the supernatant liquid through a very fine filter paper. Label
6 i% a$ P' K' { u2 [the filtrate Sample Solution B.
5 _5 d/ m. z: g" nSample Solution C8 |0 b6 t( k! u% j$ h# e) x6 M
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
5 J+ b; ~/ ~! [/ J! o/ t$ q4 R: m8 l& q, Tflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
$ k& \+ \$ \4 p( Q2 gsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.023 O. U% ]4 l) x1 z$ b6 h6 u' y0 ~
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
% i+ O% M' U+ V4 q" Z6 nknown, calculate the optimum volume of EDTA solution to be added
- D- ~0 e6 `1 M# p) w6 t ]by the formula: (4 x % Al2O3) + 5.]
6 F/ q ~3 u& v4 o( T1 V- aAdd, dropwise, ammonia solution (1 in 5) until the colour is just
4 D6 b( x3 D( w5 w0 m1 lcompletely changed from red to orange-yellow. Then add10 ml each
* c* R6 ~/ g* _of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
2 [ t7 @5 V: w# K! rroom temperature in a stream of running water, add 3 drops of xylenol0 V( j, V s. |) Z
orange TS, and mix. If the solution is purple, yellow-brown, or pink,3 P8 L! V& I1 A& H$ d
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired& [# X, U) ~+ k/ {" }6 _& W
pH, a pink colour indicates that not enough of the EDTA solution has$ u6 l( _& @0 Z! Y8 i
been added, in which case, discard the solution and repeat this: U3 W* A7 S* k# }2 K
procedure with another 100 ml of Sample Solution B, using 50 ml,2 @1 z4 a% k8 v E
rather than 25 ml, of 0.02 M disodium EDTA.
! G9 `2 Y$ |/ A- v- \* tProcedure' D) \& l' I3 r5 F* s% J
Using the standardized zinc sulfate solution as titrant, titrate Sample
! s& Q( m2 H; ?Solution C to the first yellow-brown or pink end-point that persists for
2 ]( N! `, v: a. k9 Y% |% _% k5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first7 m# Y1 ^4 |; @- j) n! C
titration should require more than 8 ml of titrant, but for more accurate
6 m! p/ }( x- Ework a titration of 10-15 ml is desirable.
K: ~: C; y( l) c5 Z% fAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
9 V) |7 `7 x2 S5 Emin, and cool in a stream of running water. Titrate this solution, using2 ~8 J/ {# P4 b& y# F1 q. e9 `
the standardized zinc sulfate solution as titrant, to the same fugitive& n% \" n$ c$ p. K
yellow-brown or pink end-point as described above.
0 o$ v6 B: s( l3 d+ d$ PCalculation:8 B% v2 A' b3 `2 J
Calculate the percentage of aluminium oxide (Al2O3) in the sample; q3 x9 G- `/ B
taken by the formula:
4 p! O L' R& d% Al2O3 = 100 × (0.005VT)/S1 v$ ]0 z( N# h1 ?0 G) H& g
where
: R! J* P S9 J4 O$ Q" [3 SV is the number of ml of 0.01 N zinc sulfate consumed in1 d7 S- W1 ?* b L4 X
the second titration,, S; z: C O8 f" h! k/ P
T is the titre of the zinc sulfate solution,
/ `0 Q) K/ @+ a5 h! E" d4 p/ QS is the mass (g) of the sample taken, and4 I* q; ^& h+ m6 Z4 o
0.005 = 500 ml / (1000mg/g × 100 ml).
3 V, X; [+ z; sSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica+ r. x: A% k# k: F1 @5 w- N
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
% i7 D' e1 n7 T" Z# o/ d# n+ ]& H$ MHeat gently over a Meeker burner, while swirling the flask, until
9 L& W( K) N& |decomposition and fusion are complete and the melt is clear, except
8 n) p9 c8 B( \8 bfor the silica content, and then cool. (Caution: Do not overheat the' Z- K9 ]$ s6 l/ R) J
contents of the flask at the beginning, and heat cautiously during
5 U9 v" e8 ]) }fusion to avoid spattering.)
4 T( @ K6 ^ d* h- }' ?6 g ]0 RTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat9 x+ ^! j& m5 M$ i3 K
carefully and slowly until the melt is dissolved. Cool, and carefully add
6 @/ `/ j9 g. w2 p" c150 ml of water by pouring very small portions down the sides of the: S( u- z6 ^0 M+ n' ~
flask, with frequent swirling to avoid over-heating and spattering. Allow- W: S" w% y) s' I: ?
the contents of the flask to cool, and filter through fine ashless filter
# |$ ^* V; @; t9 s* Vpaper, using a 60 degree gravity funnel. Rinse out all the silica from
6 S) n( j" z, u. z+ L) o. x `the flask onto the filter paper with sulfuric acid solution (1 in 10)., J! k3 h! O1 N$ m) K& E+ m
Transfer the filter paper and its contents into a platinum crucible, dry in% l* m0 }/ ^5 K6 R
an oven at 1200, and heat the partly covered crucible over a Bunsen
8 w4 H; }+ e2 Q1 J- R& d$ b8 Gburner. To prevent flaming of the filter paper, first heat the cover from4 }( i8 J- y" S, _* x; z: [/ n
above, and then the crucible from below.; g7 A) Z; b$ N6 `/ ~
When the filter paper is consumed, transfer the crucible to a muffle% \. _& I% ~0 K
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
( F( h6 d/ [0 P( S2 dweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated" \* u7 ?/ C/ }/ Y
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first2 g! P0 _# Y; y3 \
on a low-heat hot plate (to remove the HF) and then over a Bunsen) G/ F( @4 |- d- }* s+ o
burner (to remove the H2SO4). Take precautions to avoid spattering,1 Q$ Z/ f. n }6 k
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a/ _+ W# A9 K0 d# r4 p" L
desiccator, and weigh again. Record the difference between the two
/ M: w9 {4 k9 V4 J8 I! R6 Q) L6 uweights as the content of SiO2 in the sample.9 P, f5 M# j7 L9 }7 e; Y5 W
METHOD OF ASSAY8 U( ~/ i/ |/ l3 ]: n" [
Accurately weigh about 150 mg of the sample, previously dried at 105o+ P7 Q9 l3 M( o! ] ]0 m
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water: ]+ @4 Q3 U( X8 {: p
and shake until a homogeneous, milky suspension is obtained. Add 30% T( C# G6 G8 v7 p* l4 @* u. \2 \1 j
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially" `" \1 u* l. @9 K0 v1 L4 y! G
heat gently, then heat strongly until a clear solution is obtained. Cool,
. B' P/ e5 i) K/ _& r3 zthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
+ c7 D* j5 d+ z6 cacid, and stir. Add 3 g of aluminium metal, and immediately insert a
* S5 Z$ L/ W7 jrubber stopper fitted with a U-shaped glass tube while immersing the
7 K' Q7 k; o4 g: V4 A) u0 Eother end of the U-tube into a saturated solution of sodium
: Z' o4 D) w6 V0 |% _6 z( A. [3 @bicarbonate contained in a 500-ml wide-mouth bottle, and generate. i+ Z/ R( A4 C- [; G# Y, d) E
hydrogen. Allow to stand for a few minutes after the aluminium metal
3 M. G& {8 d5 d4 P% f2 Jhas dissolved completely to produce a transparent purple solution.' _' O3 I' O, s* @2 w
Cool to below 50o in running water, and remove the rubber stopper6 o0 r7 w6 s2 }: w. Q3 Y
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
, r+ j, {! N. `9 bsolution as an indicator, and immediately titrate with 0.2 N ferric
0 r/ Q" r4 B% W: o4 h Cammonium sulfate until a faint brown colour that persists for 30
7 L: M* ]5 a* I# @/ `( Zseconds is obtained. Perform a blank determination and make any& o/ n3 _. M0 {% Y5 }: [- ^
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
|9 H; i' k' v7 ?" r1 {equivalent to 7.990 mg of TiO2.
, M1 M* q" V8 M) j5 s% ~ |
|