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二氧化钛(钛白粉)
二氧化钛(钛白粉)
: R, U1 O) h3 E' e
2 z- i. j* R3 N0 ~- CJECFA关于二氧化钛(钛白粉)的结论
, Y$ o1 I" y2 i& b
! M8 q" s7 K" \2 ]$ R摘要: 2006年JECFA关于二氧化钛的结论
! j) Q! Y. l2 C4 {9 R5 lADI值:不作限制。
0 J% x2 v5 f$ T" z/ ^9 o功能:着色剂
. r4 v2 G5 A: I. Y# N7 z
( T) M; h& o( qTITANIUM DIOXIDE
I" }/ S. E% ]9 H9 }3 j5 i8 hPrepared at the 67th JECFA (2006) and published in FAO JECFA) W6 s/ k" g- [$ B# P
Monographs 3 (2006), superseding specifications prepared at the 63rd
+ y- H2 @. u5 d" ~7 e$ IJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
# ~) |# H0 [) l3 m: BCombined Compendium of Food Additive Specifications, FAO JECFA G! ?% b6 D8 G) A- @3 v' \* x
Monographs 1 (2005). An ADI “not limited” was established at the 13th+ G: ^! B+ h t* C" ~/ a! K
JECFA (1969).
. |4 C+ a6 w2 X$ Y3 Y2 v/ `$ sSYNONYMS; @3 p( c! t+ s7 |) j
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
! n9 Y8 n& B. v: u* Y GDEFINITION
Z: G8 U+ `) uTitanium dioxide is produced by either the sulfate or the chloride
\: I8 G1 w5 s, \- Z- c* l$ j8 s& fprocess. Processing conditions determine the form (anatase or rutile6 m5 T7 ]- s0 M. K* g n% A
structure) of the final product.. I+ N% b+ |# f2 F: V& {
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
# @8 |4 g |5 `( M7 Ror ilmenite and titanium slag. After a series of purification steps, the2 }5 i" t# w5 v, ^+ ~9 r! Q
isolated titanium dioxide is finally washed with water, calcined, and. M0 o' L/ B- |" o2 @9 ~: F
micronized.6 l& I1 E8 u, A* \! L
In the chloride process, chlorine gas is reacted with a titaniumcontaining" f/ q: u: T2 [, ]9 Y
mineral under reducing conditions to form anhydrous
) N! j9 d h; o- ctitanium tetrachloride, which is subsequently purified and converted to
/ t2 J, }$ O! a6 j. {% |, {titanium dioxide either by direct thermal oxidation or by reaction with
" \" n: V" F R! h* rsteam in the vapour phase. Alternatively, concentrated hydrochloric7 P' u- O1 G9 q; m. _
acid can be reacted with the titanium-containing mineral to form a
: B. u# z+ F: z) l B" ~0 }& isolution of titanium tetrachloride, which is then further purified and
3 B2 d9 J. l0 P" v0 s5 T2 W2 r" }converted to titanium dioxide by hydrolysis. The titanium dioxide is
4 G6 w. d0 u6 i4 U5 z% L3 U" W& Efiltered, washed, and calcined.
+ s' l! D: g% ~/ S2 nCommercial titanium dioxide may be coated with small amounts of' K3 {4 e7 a, ^; n& m
alumina and/or silica to improve the technological properties of the
! A% h: h" E' u3 {) r5 a* Bproduct./ a! r. `9 O$ K2 B0 X8 [+ k. P
C.A.S. number 13463-67-7
1 r) p- Y/ P" B( K& ^5 Q0 s- AChemical formula TiO2: X- n- h2 c: V: R9 B5 c9 I
Formula weight% |0 `- j- }$ B' B5 i0 C3 L
79.88" M* e% k b& n( t; K8 a
Assay) ]" {! O% I2 C; C O- O2 {# s
Not less than 99.0% on the dried basis (on an aluminium oxide and
- W2 w7 M% e5 ?! K; \8 gsilicon dioxide-free basis). h3 [. V( a. X5 h7 p' Q M
DESCRIPTION
6 v3 R0 g: O' i! l$ N) SWhite to slightly coloured powder7 }3 S7 K8 {3 m: d" y- I
FUNCTIONAL USES# P8 s3 L# `2 P: o; R/ X$ i
Colour8 o$ T" \8 C2 b( B5 q* P
CHARACTERISTICS& n6 n( K% G5 _2 @% A/ q8 q
IDENTIFICATION
' k" Y$ z) ?- `9 p U( ~( dSolubility (Vol. 4)
; G/ B# p1 X1 Z% ~0 i$ ]" ZInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
- v, t% S5 }' u4 E, n3 C" Asolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
* ]+ e7 c7 L+ f$ K8 ?) x; bsulfuric acid.
2 T4 t8 l [3 y# fColour reaction
& M" G. E; ]2 X9 CAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
0 X( j( j/ o+ U' v1 \sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
. @2 Z6 A$ A5 H; S) h. d% twater and filter. To 5 ml of this clear filtrate, add a few drops of
+ D0 U6 K1 N! m5 \4 \% @hydrogen peroxide; an orange-red colour appears immediately." e: f: D8 f' H/ \7 _
PURITY3 C; g! ]2 u5 ~0 {
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
' H4 r; p5 C- V0 d: sLoss on ignition (Vol. 4)
8 n2 {/ k2 h$ Q4 a) `Not more than 1.0% (800o) on the dried basis
! V2 }; T& v' l: o7 G1 n# [Aluminium oxide and/or7 D9 v" U- I" }9 a
silicon dioxide
* ^* n8 l% m/ c" N' o7 ^Not more than 2%, either singly or combined# L k7 T, x+ D. h+ I4 p7 n" g" i
See descriptions under TESTS$ J8 i5 J( k. @5 f
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing }: y, T( v n! Z. T
alumina or silica.0 j7 c% V. j7 U6 U/ ~
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and8 t7 v9 A% o/ [0 d- H
place on a steam bath for 30 min with occasional stirring. Filter( `, x* \; ~% ^- M. j
through a Gooch crucible fitted with a glass fibre filter paper. Wash
! K9 r+ D6 r. iwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the6 B- j! A/ W- K* v5 f
combined filtrate and washings to dryness, and ignite at a dull red
6 O5 @9 F1 w$ B) K( R4 Fheat to constant weight.
/ M, j2 _7 [, G Z6 _Water-soluble matter
0 k$ `0 M. F! O6 M' p4 c! O8 S. q/ S(Vol. 4)* K3 F$ v0 m3 X& h0 n5 k
Not more than 0.5%
: }% z. b! {- k, p! [Proceed as directed under acid-soluble substances (above), using9 h$ T( x& l# t; U
water in place of 0.5 N hydrochloric acid.& r4 g" N9 i2 x; K8 v
Impurities soluble in 0.5 N) t1 E5 a7 U8 N3 T* h7 l: B/ C* m
hydrochloric acid% A+ }" y/ X' I$ C
Antimony Not more than 2 mg/kg. @$ ?$ g6 n- |6 V2 @( N! G& D
See description under TESTS
3 d$ h6 C( |7 {- @Arsenic Not more than 1 mg/kg5 l/ V0 y) o s' X& ^
See description under TESTS) }2 V3 y7 Z3 Z! J1 ]8 c/ ]% n
Cadmium Not more than 1 mg/kg
$ k. g) c. u$ ~/ mSee description under TESTS
1 f7 H4 F5 B! Y6 g4 |; v! GLead
& m6 N. Y- d" g ~% K, \/ n3 aNot more than 10 mg/kg
$ b8 H# G- c3 d2 y g. X9 kSee description under TESTS. L" F" o/ h+ D
Mercury (Vol. 4) Not more than 1 mg/kg0 S/ M Y/ A; Z3 t) N R
Determine using the cold vapour atomic absorption technique. Select a: h- x1 p9 ?7 T) E2 W
sample size appropriate to the specified level
, l' m& {2 K& o4 ]! s; }) UTESTS
: e# ]+ I2 I" S* U/ bPURITY TESTS
. ^( l' j4 B7 t$ S: j- [: j! eImpurities soluble in 0.5 N
2 O. y2 _: D( r/ x* ohydrochloric acid
2 T) M8 Z- ?- p7 [% ~8 f+ }5 rAntimony, arsenic,+ L2 s) S/ v1 Z5 s+ `# Z
cadmium and lead
' M) c* H$ }9 @(Vol.4)
/ b: y3 O3 L: _Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
1 M, w; \* C& G# Thydrochloric acid, cover with a watch glass, and heat to boiling on a5 d/ Y) A4 S6 H1 b
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
# f+ h6 ^' [' L4 h7 e! bcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved" b( L/ W" c k" X i
material settles. Decant the supernatant extract through a Whatman6 s1 {/ y$ f+ \$ P+ K( k
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
* ^6 L& s) J5 Yvolumetric flask and retaining as much as possible of the undissolved
" }" W' Z9 ?2 N* O" B* ematerial in the centrifuge bottle. Add 10 ml of hot water to the original ?: v& h9 q F+ r- l2 D3 N
beaker, washing off the watch glass with the water, and pour the
e) w j% o3 Ncontents into the centrifuge bottle. Form a slurry, using a glass stirring
2 F. A4 c* v; R; V. J8 yrod, and centrifuge. Decant through the same filter paper, and collect
7 l+ \& }0 c0 jthe washings in the volumetric flask containing the initial extract.
# u8 d$ C& C2 n8 ~7 W/ VRepeat the entire washing process two more times. Finally, wash the- k5 \- `" v% d- X4 V2 I
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask" i/ Q( [9 O. j8 I
to room temperature, dilute to volume with water, and mix.; {. J: s. I" [ @
Determine antimony, cadmium, and lead using an AAS/ICP-AES @, V7 M( ^, J4 P# V, \
technique appropriate to the specified level. Determine arsenic using the. r' d& D n! A B5 n' ^
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
# O+ q" L+ h$ j+ y7 _2 c4 iMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
, Q8 T) R8 X. F: ~: Y0 F1 g. The selection of sample size and method of sample preparation
g* U2 [8 k3 k: pmay be based on the principles of the methods described in Volume 4.
0 I/ I* r7 A% v% r/ \Aluminium oxide Reagents and sample solutions
6 K1 e8 ~8 }; \3 l: f, R7 V0.01 N Zinc Sulfate c% |$ [! F) Q1 A+ `9 l: |
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
; |3 O# y" V) L( y1 Bmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg) y& _6 T2 A9 k
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
6 n3 e' ]9 ?( O9 ^ o8 A& wconcentrated hydrochloric acid, heating gently to effect solution, then/ [3 W& J/ v/ ^! I
transfer the solution into a 1000-ml volumetric flask, dilute to volume+ O' J' _+ a, P# o
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500; h4 v) U1 j: A; n4 \( U) U
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
% y2 C; a7 R! O/ \* bconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
- U% O9 U' e+ t1 L Y25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
* e# f! M0 k" e0 `" _2 odropwise, ammonia solution (1 in 5) until the colour is just completely. @7 n' ]5 u3 O7 W
changed from red to orange-yellow. Then, add:
; i! f' s9 R0 P: I, {# {! V(a): 10 ml of ammonium acetate buffer solution (77 g of
- g5 k) c) X. X& D2 d [+ H. H* nammonium acetate plus 10 ml of glacial acetic acid, dilute to
3 N# B* _; p C' B( d5 [1000 ml with water) and
0 w, J" @$ u. G% m(b): 10 ml of diammonium hydrogen phosphate solution (150 g, Y6 f- Z# N- s/ L4 T
of diammonium hydrogen phosphate in 700 ml of water,6 H. U2 V0 j# q, p9 \
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,! R) R9 D# O6 O, _3 P
then dilute to 1000 ml with water).
1 q, b+ b- {$ r K$ s* Y0 s0 CBoil the solution for 5 min, cool it quickly to room temperature in a
1 R/ p5 @1 U% v, y) B7 Pstream of running water, add 3 drops of xylenol orange TS, and mix.5 \+ x) U# V+ l0 f# ~5 i1 @9 Y
Using the zinc sulfate solution as titrant, titrate the solution to the first
3 z. b. t) {+ X; Byellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
0 d. u. D- s; G5 z5 u: tThis titration should be performed quickly near the end-point by9 J; P: ]& Q% z7 \# M
adding rapidly 0.2 ml increments of the titrant until the first colour# C( b, h9 {8 `
change occurs; although the colour will fade in 5-10 sec, it is the true
3 i) G. u1 `0 p% O( Z. b( R" k& Gend-point. Failure to observe the first colour change will result in an! z, {+ b! g! ~! A# C
incorrect titration. The fading end-point does not occur at the second
2 y) W5 M/ c1 M. r% O# i& pend-point.)
9 ]& E9 }1 J8 D: K- ~Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a* N* u% _1 j8 `8 P) y# S- g4 k
stream of running water. Titrate this solution, using the zinc sulfate
# b) |2 g8 ^. m0 f+ j3 z( asolution as titrant, to the same fugitive yellow-brown or pink end-point7 s& q) h% ? X4 ?; @+ a x
as described above.# A, P8 `' y) k' y5 L& d4 r
Calculate the titre T of zinc sulfate solution by the formula:: {* d! P$ }, l5 S, Q9 N
T = 18.896 W / V% ]3 W7 Q% r E- t z9 p
where
$ f1 m; r3 P1 f" {7 U7 {T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
3 g& u# L& a v+ ~$ gW is the mass (g) of aluminium wire/ W* M$ N! H4 e
V is the ml of the zinc sulfate solution consumed in the
& o# z" o1 x7 ?second titration% `. y: y( `4 `
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and7 J: O- [( Z k2 |6 U) g2 }& K
R is the ratio of the formula weight of aluminium oxide to
# H) |+ f. X( G" p2 O7 Vthat of elemental aluminium., D$ H. D5 V& R2 S
Sample Solution A
7 Q2 |% |- e" {0 FAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica7 P- H9 j& R1 O& h/ M: |
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
9 @% t% w- `6 w0 G0 p- d(Note: Do not use more sodium bisulfate than specified, as an excess
% p( t' d" d8 N$ vconcentration of salt will interfere with the EDTA titration later on in the8 l5 p3 m: G- L8 S8 u. Q0 G( h! L
procedure.) Begin heating the flask at low heat on a hot plate, and) F3 J0 e" I. \4 A
then gradually raise the temperature until full heat is reached.2 o9 j' S% A7 o% m6 F+ k
(Caution: perform this procedure in a well ventilated area. ) When0 A6 r t1 y: g' e1 u5 M( i: f
spattering has stopped and light fumes of SO3 appear, heat in the full3 {3 v8 `2 G( X% c! u8 z0 U- X7 v
flame of a Meeker burner, with the flask tilted so that the fusion of the; [! O. T1 A( s3 R9 C: \% D
sample and sodium bisulfate is concentrated at one end of the flask.
' e. I8 i3 T, P% WSwirl constantly until the melt is clear (except for silica content), but H& e$ D1 O( U+ D1 T
guard against prolonged heating to avoid precipitation of titanium
" v: X) W. Q0 p0 Edioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
0 S( X0 }/ l& Y5 V# b) a$ [; lthe mass has dissolved and a clear solution results. Cool, and dilute to
; Q: }0 h8 S7 |$ t# ~120 ml with water. Introduce a magnetic stir bar into the flask.8 n/ z+ o- L" n2 O* b! p; f8 M
Sample Solution B
+ A: x! a3 \, h( D% e/ m4 gPrepare 200 ml of an approximately 6.25 M solution of sodium# ~: G% G; I0 j* Z! T" |
hydroxide. Add 65 ml of this solution to Sample Solution A, while0 y ]5 J) G2 O5 i1 d. D+ F
stirring with the magnetic stirrer; pour the remaining 135 ml of the
+ x6 e. e$ w1 Z2 a9 a6 malkali solution into a 500-ml volumetric flask.3 x% o" Q2 Y0 y+ ^0 s
Slowly, with constant stirring, add the sample mixture to the alkali
& B, l9 W( x5 x1 {8 Msolution in the 500-ml volumetric flask; dilute to volume with water,
$ X. ~6 { M/ \% K0 H4 o) ]: o+ M+ Gand mix. (Note: If the procedure is delayed at this point for more than! A$ R- l+ Y; G3 a3 ^, F3 m/ s/ ?
2 hours, store the contents of the volumetric flask in a polyethylene% |$ b. b7 f$ ~4 ^# F9 \3 }1 o3 ?
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),5 b/ h. w1 o5 m4 P4 M6 H4 q
then filter the supernatant liquid through a very fine filter paper. Label
! d2 ^' j! D9 `. X& ?3 kthe filtrate Sample Solution B.* q& P! I7 Q7 k, n" B
Sample Solution C
1 B( Y2 u! Z& {3 }9 P, X6 jTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer6 t: U h I) D' R. M. ~
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
0 X0 w! b+ o: z& ysolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
1 @2 g g8 g7 n2 K9 G0 W0 IM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
# J, M1 ]% B6 e7 l* u* \known, calculate the optimum volume of EDTA solution to be added
9 N/ w; O% Y' j" [' x" S+ Sby the formula: (4 x % Al2O3) + 5.]
8 J2 b. Y8 p' [8 _' CAdd, dropwise, ammonia solution (1 in 5) until the colour is just
& t7 @" G- w/ b6 `& }completely changed from red to orange-yellow. Then add10 ml each' L( `" J- Y. `( R, r0 ^* P
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
& c5 }, ]! C6 C* Q" Rroom temperature in a stream of running water, add 3 drops of xylenol
4 H) d M2 j0 ~( r8 @$ Porange TS, and mix. If the solution is purple, yellow-brown, or pink,
6 i0 a* C f6 V" Fbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
7 U2 F" \" J: L* r* {/ f3 h IpH, a pink colour indicates that not enough of the EDTA solution has
, h9 U0 S5 t+ l8 \+ v' abeen added, in which case, discard the solution and repeat this
, D& k6 M& h1 Y: f! g8 M }/ J3 tprocedure with another 100 ml of Sample Solution B, using 50 ml,
( [+ q) {; e! @3 y5 b# e1 O7 Qrather than 25 ml, of 0.02 M disodium EDTA.
" p/ G3 Y* K" d7 b {Procedure
- }+ I: Y$ _6 m2 \/ dUsing the standardized zinc sulfate solution as titrant, titrate Sample
" u5 `5 D* Q2 @ ]Solution C to the first yellow-brown or pink end-point that persists for, z* Y7 j: s7 [& Q5 L8 y( H; c7 S3 A
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first# x/ q2 C6 \ F9 B- y7 D; m, ]: I$ H
titration should require more than 8 ml of titrant, but for more accurate& S6 K! ^! |( x7 Q( k" U8 j
work a titration of 10-15 ml is desirable.
+ y: Q6 E* I E- i: RAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
; L7 H. v+ j S! wmin, and cool in a stream of running water. Titrate this solution, using4 N' v( D0 r" p( @% u2 a0 w+ J
the standardized zinc sulfate solution as titrant, to the same fugitive
' @) O0 C: U0 I. }yellow-brown or pink end-point as described above.8 C$ W5 b- E. [% u3 x" X
Calculation:
0 P( k& g: S0 R1 c0 y# T# MCalculate the percentage of aluminium oxide (Al2O3) in the sample& r, @" ~0 p2 ]& N* \ G$ o6 H
taken by the formula:
, E; X7 f; G6 J7 j% Al2O3 = 100 × (0.005VT)/S
% L- v+ }: f" \+ w+ @! y" ?7 {+ Mwhere
! n$ Q' u; n- O+ F2 ~: b; _% `* U- K* AV is the number of ml of 0.01 N zinc sulfate consumed in
: F5 X8 k2 A4 V# `5 mthe second titration,5 I( v! {6 K% v1 |0 c$ y+ y. p" N
T is the titre of the zinc sulfate solution,
7 }! B! n3 z) S# {! u0 PS is the mass (g) of the sample taken, and! t2 i1 Y4 s w: ~( v
0.005 = 500 ml / (1000mg/g × 100 ml).
) D! w0 |6 Z4 H( uSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica, Y" ~6 R: H: G& y" m% \
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).1 {6 j, u/ q6 S
Heat gently over a Meeker burner, while swirling the flask, until
$ I( M9 d- j% M! T' r8 O' hdecomposition and fusion are complete and the melt is clear, except; e' c! H4 W# }4 i0 Q
for the silica content, and then cool. (Caution: Do not overheat the: F3 k$ m* Q! l6 }1 X r
contents of the flask at the beginning, and heat cautiously during
* z% ] L! Y* j. q, k5 efusion to avoid spattering.). H3 m! d$ n; I& M3 i0 e! b8 f! d
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
% {% w' C3 Q, W" \) `- _carefully and slowly until the melt is dissolved. Cool, and carefully add
7 @1 Q) x, `$ k% M8 H! {150 ml of water by pouring very small portions down the sides of the0 c! `9 @7 v( n. m1 ]& i9 c& V
flask, with frequent swirling to avoid over-heating and spattering. Allow
1 N# P3 \1 L& Zthe contents of the flask to cool, and filter through fine ashless filter
+ m8 {! }2 B0 a1 y- f1 u0 M) Zpaper, using a 60 degree gravity funnel. Rinse out all the silica from1 E3 f% j# B/ o. @0 U$ q5 s
the flask onto the filter paper with sulfuric acid solution (1 in 10).
4 ?7 ~: [$ O3 C9 x$ m( h( wTransfer the filter paper and its contents into a platinum crucible, dry in
7 G6 y9 ]: L& C, Y& yan oven at 1200, and heat the partly covered crucible over a Bunsen3 e" V8 b! U" C5 o/ ~# S
burner. To prevent flaming of the filter paper, first heat the cover from
F, `8 A1 v4 N8 p% [above, and then the crucible from below.) G* U. z, Q8 o( F6 I
When the filter paper is consumed, transfer the crucible to a muffle
( y- x8 y$ V6 p6 H' Rfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
7 l- `4 [ k$ I6 \8 T" F0 Rweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated+ @. ~+ R6 h8 A: Z* L
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
# E; b( g5 p0 k$ J: D, S5 Hon a low-heat hot plate (to remove the HF) and then over a Bunsen& v. I2 H- }% V/ ]1 L* g
burner (to remove the H2SO4). Take precautions to avoid spattering,2 D0 n4 n( v' W o
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
7 M7 I9 k, r1 Cdesiccator, and weigh again. Record the difference between the two
+ ~8 ?% b# n4 V9 U$ jweights as the content of SiO2 in the sample.+ I, e' G( S9 o$ P1 t) Z
METHOD OF ASSAY0 U$ b: T1 F5 F, _+ {
Accurately weigh about 150 mg of the sample, previously dried at 105o8 I. S1 P3 w& x S; ~0 X/ M) W
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water* v2 g3 K2 P3 I6 {1 M7 `" A
and shake until a homogeneous, milky suspension is obtained. Add 307 u* H7 |$ Z! m, M" k
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially! [; |/ A9 d, s, {
heat gently, then heat strongly until a clear solution is obtained. Cool,
! t/ b! }: x3 d6 A/ Y* ?then cautiously dilute with 120 ml of water and 40 ml of hydrochloric# l4 n( a6 }0 W; M
acid, and stir. Add 3 g of aluminium metal, and immediately insert a8 H( o2 b) X+ p. {) y
rubber stopper fitted with a U-shaped glass tube while immersing the
0 F2 j# S* @1 ]: F6 d6 u7 Dother end of the U-tube into a saturated solution of sodium, ?$ ~0 w# e* p$ Q. p
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
( L" Y- W1 F& e( h( Shydrogen. Allow to stand for a few minutes after the aluminium metal
! p' K: ]% y: t7 ~has dissolved completely to produce a transparent purple solution.
+ Y9 m+ @" n0 w& `$ v/ V2 UCool to below 50o in running water, and remove the rubber stopper
- U8 N9 j6 Z, c( E3 ycarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
! H( T6 }/ X+ H: }1 Msolution as an indicator, and immediately titrate with 0.2 N ferric. D# {* x* L% H7 i
ammonium sulfate until a faint brown colour that persists for 30
1 |) F" V& F2 B5 T9 L9 [seconds is obtained. Perform a blank determination and make any4 S, D1 z) ^ O* [
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
6 ~- x1 S" J! I6 F! Q5 bequivalent to 7.990 mg of TiO2.
% a8 d1 ~ U) ^/ Y, _, Y7 f; D6 l |
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