|
沙发

楼主 |
发表于 2008-5-23 12:10:00
|
只看该作者
二氧化钛(钛白粉)
二氧化钛(钛白粉)
: D4 Q" a7 {! H" d _: H% D" C9 B
JECFA关于二氧化钛(钛白粉)的结论
% ^; [! k- P1 f3 @/ t; _% ?) V( O5 h
p& {' {; @# v c( `摘要: 2006年JECFA关于二氧化钛的结论
; `% h' i# X' O, G- qADI值:不作限制。 L7 X3 ]9 T" ^0 Z" q8 Q
功能:着色剂
# o1 V' N- e: u
4 e6 a6 d& D+ f* Y+ i( \8 D) WTITANIUM DIOXIDE
3 a& O% O! X& |+ O; ePrepared at the 67th JECFA (2006) and published in FAO JECFA- m- ~2 u$ n# G' \! V2 m J/ j
Monographs 3 (2006), superseding specifications prepared at the 63rd7 C: K* f% m+ N" {) ` _
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the, l9 b: x3 G9 w2 i# x$ T
Combined Compendium of Food Additive Specifications, FAO JECFA
: ?' K- A! O: a- m% `- bMonographs 1 (2005). An ADI “not limited” was established at the 13th1 V, @/ g! D, L1 ?( Q
JECFA (1969).0 g J1 u& I& G/ v3 I. [# f, b
SYNONYMS- x2 O. W$ L& L0 _
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
; j! d6 h! p9 g! yDEFINITION
) \# K. e/ x W' _Titanium dioxide is produced by either the sulfate or the chloride# J/ x. q7 d5 A) w
process. Processing conditions determine the form (anatase or rutile
. f! u* P- |+ P& c4 F1 o4 }) Q) A! o/ k0 @structure) of the final product.
' u& C7 z- U1 n% J9 ]- r& mIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)3 w! ~, ^5 Z+ |: K1 Z5 T+ m
or ilmenite and titanium slag. After a series of purification steps, the
* g8 z _' o& W& A1 Y7 _ ~3 zisolated titanium dioxide is finally washed with water, calcined, and' F. x3 B& Z! ^3 w& a) h' S
micronized.7 c2 ~+ Y. d+ ^2 h
In the chloride process, chlorine gas is reacted with a titaniumcontaining- I# R6 R( L _6 N
mineral under reducing conditions to form anhydrous, G6 N1 i1 I( c2 K
titanium tetrachloride, which is subsequently purified and converted to
( G4 |6 G0 }3 ~# F0 d, E- atitanium dioxide either by direct thermal oxidation or by reaction with
8 h& G! g( U5 z. h7 Ssteam in the vapour phase. Alternatively, concentrated hydrochloric
7 {; I7 s8 v$ I: D8 nacid can be reacted with the titanium-containing mineral to form a
3 L5 E+ v. `' s0 Psolution of titanium tetrachloride, which is then further purified and
* `5 e L' f8 M4 G# hconverted to titanium dioxide by hydrolysis. The titanium dioxide is7 A% D8 n r" j) u
filtered, washed, and calcined.4 P2 }) z7 B) R6 o) e
Commercial titanium dioxide may be coated with small amounts of
9 V J2 o- B7 M, U* p' Malumina and/or silica to improve the technological properties of the
. T7 G, T$ B5 B* aproduct.2 n( E' q* Y" O5 m
C.A.S. number 13463-67-7
- F+ U' r: H) ?7 A% `5 l4 h8 kChemical formula TiO2
( A$ V. P3 R* c, _0 x2 {Formula weight' F& p! ^+ E# A" E3 F) `( f$ q
79.889 h! b( @; N7 u8 D
Assay. Y- X7 |$ r) e) ^% E* M( D
Not less than 99.0% on the dried basis (on an aluminium oxide and7 v) {6 \8 L. v7 v: L! C' j) E% T- ]
silicon dioxide-free basis)5 w' W! @6 ]8 U. V
DESCRIPTION6 a* x3 T5 [5 C1 ^# \$ Y
White to slightly coloured powder
1 y0 ]( F' l! @, J6 T% q5 l$ VFUNCTIONAL USES. w# d/ x1 `% `
Colour- \, u0 c+ f# d* B) C* Q) H0 E% B
CHARACTERISTICS
+ E$ |9 N8 J3 @! ` o6 T; gIDENTIFICATION
; a% L5 }; Y( v6 USolubility (Vol. 4)
3 r/ [ n+ ]' B2 y0 B' Z8 CInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
+ E+ s u* ?( g: y* K+ H# zsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated1 v' L" i( m3 R8 [. s
sulfuric acid./ w: W$ ^" \8 L
Colour reaction$ ]3 a3 S" p7 ?7 E3 X6 Z- X6 t
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
4 v+ o0 G W! u- N/ Z8 ysulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
- R2 w( g( Y5 R! T& awater and filter. To 5 ml of this clear filtrate, add a few drops of
! u5 G) h, ]5 s& [+ `hydrogen peroxide; an orange-red colour appears immediately.* D* u. m' I& G
PURITY
. R7 R1 Z& O+ j$ b$ m- gLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
) L* B4 ~3 E, j5 NLoss on ignition (Vol. 4)3 ]1 L) F$ Y! R# d+ P$ u
Not more than 1.0% (800o) on the dried basis
0 p& a( l8 J7 _& j0 l8 B* U; @Aluminium oxide and/or: H" b1 E! w; U: d# Z
silicon dioxide
9 [4 o# I7 `9 s' H0 R) J; ?Not more than 2%, either singly or combined
; Q0 b! g! u( o& KSee descriptions under TESTS- k2 X, ^: y* t. _
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
. S5 w! c: Q" Halumina or silica.
) z* a# H% t5 m1 V, B, Q' D: sSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and! w% x% C6 v8 [0 x6 q
place on a steam bath for 30 min with occasional stirring. Filter7 r6 r$ C) c4 _7 i
through a Gooch crucible fitted with a glass fibre filter paper. Wash _' f, G5 P% r/ g! z6 ?
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the1 w2 @* T0 ~2 A; y/ X1 K0 M6 ^
combined filtrate and washings to dryness, and ignite at a dull red1 |6 J2 t& c+ S5 T t t
heat to constant weight.+ U* J5 h3 A. C, r* b) \
Water-soluble matter
; C- y3 t7 A2 ^) H4 f(Vol. 4)
7 B r2 `: ]+ ^* \Not more than 0.5%
. w9 @# _4 u9 QProceed as directed under acid-soluble substances (above), using
2 N6 a6 J% j; B- N. m: `water in place of 0.5 N hydrochloric acid.
, O6 q% i3 O- ?9 c8 W+ d- XImpurities soluble in 0.5 N# j% \: K" z4 Z- s+ o
hydrochloric acid
2 D4 x% E: r% [& bAntimony Not more than 2 mg/kg7 W9 d# D- v0 U4 ~5 b
See description under TESTS. T: M! k [- s7 f5 D; m
Arsenic Not more than 1 mg/kg, t0 |, u+ L ]3 {' g
See description under TESTS
- d& \ c" T! G2 S' k D$ l" eCadmium Not more than 1 mg/kg
, U! d/ x7 C, ^) bSee description under TESTS
" n$ I4 ~0 a% W! ~: Q. r2 a% ~1 lLead
" l |! ~0 Q1 _3 I( tNot more than 10 mg/kg/ S! L3 O k8 c y. B/ F
See description under TESTS# a" s9 u4 G6 b& Z' r4 Z
Mercury (Vol. 4) Not more than 1 mg/kg
' H/ K. H* ^& W1 X" |& ZDetermine using the cold vapour atomic absorption technique. Select a( f1 \; R' S& m' Z+ Y+ p! x
sample size appropriate to the specified level( `! O* g* G, B, ]
TESTS6 N! b2 {9 q7 l5 v4 n) j( S4 Z
PURITY TESTS6 [7 |( I% `6 ~' ?# D- s" Y
Impurities soluble in 0.5 N
: k* m0 E+ e: S Y$ lhydrochloric acid; }6 ^8 b# {! D; q+ G. e* }
Antimony, arsenic,
' ]0 f; m! j" Z9 O4 f. Gcadmium and lead1 H5 z( T4 q2 Z% N, v5 w0 s v
(Vol.4). ^8 z8 I* C& M5 S
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
' V; L) f+ Q( Nhydrochloric acid, cover with a watch glass, and heat to boiling on a! d/ e" u' X4 I5 S. Q
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
9 T- A% U! P. qcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
* v: v) L6 T2 z3 Y, dmaterial settles. Decant the supernatant extract through a Whatman. H. n3 P) g, R" |1 H& Y
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml6 ~4 f% v3 I( a
volumetric flask and retaining as much as possible of the undissolved' Z; y5 q# d6 z/ P: ^! Y
material in the centrifuge bottle. Add 10 ml of hot water to the original+ e( m& x$ L/ _& m
beaker, washing off the watch glass with the water, and pour the
) P; j0 s4 E4 c# s1 B3 icontents into the centrifuge bottle. Form a slurry, using a glass stirring
' ^" y, l! w( X: ?rod, and centrifuge. Decant through the same filter paper, and collect! j* t1 H7 a. X0 z: g( F/ ]( g9 x
the washings in the volumetric flask containing the initial extract.
* y" m" M3 Q, F& URepeat the entire washing process two more times. Finally, wash the" {: ]+ I3 w7 \# c, W
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
, v. h' P2 ^8 x% h+ g( J" V1 Eto room temperature, dilute to volume with water, and mix.
$ t7 R" K4 `4 x- ]( z( `8 s8 @Determine antimony, cadmium, and lead using an AAS/ICP-AES3 G) D) U' k* h6 p! e/ r a* X
technique appropriate to the specified level. Determine arsenic using the3 F: @# k, s9 \1 b
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using- [9 \: @$ ~1 g/ q. z$ i
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than- E$ L/ |* g( u [9 [
1 g. The selection of sample size and method of sample preparation8 a; R5 p# u4 @. f4 g
may be based on the principles of the methods described in Volume 4.& P! R0 ~. I: R# W4 Q# A
Aluminium oxide Reagents and sample solutions- W$ {: R; }" B6 Z3 m( U/ P
0.01 N Zinc Sulfate
- P9 s" @' R! h$ r9 W2 G& jDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to* U/ ^- C. s( ~0 i* e/ W; m
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
k1 a3 W8 a/ A" o( p5 zof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
* @/ }5 p- o' X# Nconcentrated hydrochloric acid, heating gently to effect solution, then
3 c/ Y3 [3 r3 ?9 L9 Itransfer the solution into a 1000-ml volumetric flask, dilute to volume0 M+ `" B5 E! q1 _& r
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
3 y* F) T! o3 V7 d- G( g) P$ ^ml Erlenmeyer flask containing 90 ml of water and 3 ml of
1 u( t8 o9 @& O0 { @concentrated hydrochloric acid, add 1 drop of methyl orange TS and" h( i" ^( q# N4 n+ d! s
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
+ W5 e, A/ Z% h9 S' O3 b/ n3 Jdropwise, ammonia solution (1 in 5) until the colour is just completely
2 o5 o- F- ^& b; j$ ^( Y* ychanged from red to orange-yellow. Then, add:
( A( N5 ?% E; _(a): 10 ml of ammonium acetate buffer solution (77 g of
, h* a6 N) c5 i. P/ I8 iammonium acetate plus 10 ml of glacial acetic acid, dilute to5 Z9 a$ }. r% j5 ?0 Y
1000 ml with water) and
5 ]: q; ^' u V# R( h8 s% O3 X(b): 10 ml of diammonium hydrogen phosphate solution (150 g! g, D2 k) G7 w6 F7 H
of diammonium hydrogen phosphate in 700 ml of water,
# u7 T! `9 c+ R# \ @3 P- U+ T& badjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
$ m0 r& s0 y9 p0 y% Uthen dilute to 1000 ml with water).8 g& ~1 V+ S$ g2 M+ E' M+ O
Boil the solution for 5 min, cool it quickly to room temperature in a/ W2 W' J' n+ Z" |+ r& i% p
stream of running water, add 3 drops of xylenol orange TS, and mix.- ?. u3 r4 R$ L
Using the zinc sulfate solution as titrant, titrate the solution to the first
7 F- Y$ d6 t$ n( W5 w, ^: |yellow-brown or pink end-point colour that persists for 5-10 sec. (Note: |: X' L: n/ @
This titration should be performed quickly near the end-point by
_. @* }3 R$ t" r* Kadding rapidly 0.2 ml increments of the titrant until the first colour) m) x% A' t( t; T6 ~6 M N* X
change occurs; although the colour will fade in 5-10 sec, it is the true5 Y- j' I2 y1 g7 P2 r9 m
end-point. Failure to observe the first colour change will result in an( j. {, m p0 {+ t% g" t/ ~
incorrect titration. The fading end-point does not occur at the second
3 |3 c6 }; a5 g; Y2 U$ B- t$ h- \7 lend-point.)
+ i# n* ^, F$ B5 ~Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
# Q! ]9 Z% }4 V a7 \9 E) Bstream of running water. Titrate this solution, using the zinc sulfate: }3 T3 m! U+ Q9 q
solution as titrant, to the same fugitive yellow-brown or pink end-point
5 c0 Z2 u2 A% P6 g; P) Z" R8 xas described above.
# s4 y, d9 d8 I" [1 q: S& o' cCalculate the titre T of zinc sulfate solution by the formula:
' K Q5 ]! ]$ KT = 18.896 W / V) b# l2 i6 u: n$ Z ^% j8 U# I1 f
where; A, X/ h1 ~: X3 h3 n8 A+ q
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
" \" e( {3 r4 J3 R8 K8 kW is the mass (g) of aluminium wire
: S' R/ b" Q# W1 Z q- V* ^, E" tV is the ml of the zinc sulfate solution consumed in the8 O4 _' t1 \# Q8 Z
second titration+ M9 Z' x' z" k' s0 F1 q
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and# v7 O; D) x4 l
R is the ratio of the formula weight of aluminium oxide to1 D3 t1 b; \; m+ h9 X, i" m% F4 _
that of elemental aluminium.
0 o( x ?( f! Z8 F- U, aSample Solution A6 I+ ?' M- A% Y6 n! f
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica. e) z+ e3 v% N# f2 S7 J
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).5 c4 ]- N/ _3 Q9 L$ c9 Y$ J% w8 C
(Note: Do not use more sodium bisulfate than specified, as an excess! p2 R" l- m7 U. P/ K: E
concentration of salt will interfere with the EDTA titration later on in the
8 x& h1 ~2 K* B1 I* jprocedure.) Begin heating the flask at low heat on a hot plate, and; ^8 |* `9 I3 s
then gradually raise the temperature until full heat is reached.
2 N( `4 I% T# P! Z/ D5 i$ [4 i4 x(Caution: perform this procedure in a well ventilated area. ) When
+ T3 J8 ]: x" f; \. d( Y6 ]spattering has stopped and light fumes of SO3 appear, heat in the full
/ d$ b0 t+ P: L+ ]! Q! k# [& e0 ^flame of a Meeker burner, with the flask tilted so that the fusion of the
; h$ z: Z- Z0 P& {sample and sodium bisulfate is concentrated at one end of the flask.9 R5 k8 k+ \( z5 Z4 Z
Swirl constantly until the melt is clear (except for silica content), but
+ x6 g- f; r. {* Y% R* d0 sguard against prolonged heating to avoid precipitation of titanium
$ |. \+ c5 x9 u! P' Y! Pdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
$ i7 d1 S( N: K, X! jthe mass has dissolved and a clear solution results. Cool, and dilute to
, P- o( K' L# g7 X6 k120 ml with water. Introduce a magnetic stir bar into the flask.
+ D% Z; _6 U1 V+ p7 |* }& [Sample Solution B" _" `; i' q' U. S3 {1 H: |
Prepare 200 ml of an approximately 6.25 M solution of sodium
" Y4 j. h" p0 q9 l" \! \! X# A5 Xhydroxide. Add 65 ml of this solution to Sample Solution A, while8 A; X! ?$ p" h/ {, W- o
stirring with the magnetic stirrer; pour the remaining 135 ml of the/ C( f! O ~4 \% f. ~/ K9 L
alkali solution into a 500-ml volumetric flask./ N1 x+ J3 \: q3 g
Slowly, with constant stirring, add the sample mixture to the alkali+ G8 P, c& s9 [4 S" i V* ]
solution in the 500-ml volumetric flask; dilute to volume with water,, r. r9 v; |5 l$ [
and mix. (Note: If the procedure is delayed at this point for more than
+ k, i" l% b5 q0 j: J% U2 hours, store the contents of the volumetric flask in a polyethylene
( e5 E' C& U9 r1 M A0 tbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),1 w- L a& I/ X9 u
then filter the supernatant liquid through a very fine filter paper. Label
* x$ d# y/ a8 _3 }; s7 I" ^the filtrate Sample Solution B.
, @9 ]5 R7 k a' SSample Solution C! O& N9 C/ A l% l6 j
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
4 m3 W4 r/ Z$ i; b2 Y' @flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid& D3 i! O) S* A3 h
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02) t8 B9 V- t$ h
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
2 P7 g# m" b9 e* s2 ^known, calculate the optimum volume of EDTA solution to be added
% O" j) z( @ G3 U1 D) \by the formula: (4 x % Al2O3) + 5.]
3 P2 v% b" J$ _' _9 P7 R- TAdd, dropwise, ammonia solution (1 in 5) until the colour is just# s! c2 n: V! R
completely changed from red to orange-yellow. Then add10 ml each
. l! q& ]' }$ l% }3 _! nof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
0 r- B9 ~9 P2 |4 Troom temperature in a stream of running water, add 3 drops of xylenol
I* |/ m7 w7 k: Dorange TS, and mix. If the solution is purple, yellow-brown, or pink,
" q+ Y8 |, g* R! L) U, ?* @bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired5 o5 u& V3 `8 `! z. i$ f
pH, a pink colour indicates that not enough of the EDTA solution has
/ F9 P. \& G Ebeen added, in which case, discard the solution and repeat this
# N- o+ T9 t6 R8 S5 ^; ~procedure with another 100 ml of Sample Solution B, using 50 ml," Y* @ L# j0 f
rather than 25 ml, of 0.02 M disodium EDTA.
, y6 c0 f; s, DProcedure, v; }3 E* U3 _( \" L6 U
Using the standardized zinc sulfate solution as titrant, titrate Sample9 @0 y. q! P9 q' r
Solution C to the first yellow-brown or pink end-point that persists for
) G6 y6 l3 v6 w! e2 T% [5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
) V! W3 x) y) @5 k T3 }titration should require more than 8 ml of titrant, but for more accurate
9 h$ D! N3 |( ]' f3 lwork a titration of 10-15 ml is desirable.9 [1 p4 n* i* W0 ^. \+ S
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
3 l5 d/ U% x. S- |min, and cool in a stream of running water. Titrate this solution, using" {# w- P5 K6 x( k: ]0 Y
the standardized zinc sulfate solution as titrant, to the same fugitive- @. ]' h& K. f7 O j' {, ~
yellow-brown or pink end-point as described above.0 w* K5 G$ I" [. k& C; J
Calculation:
4 o! v5 \' {# p% P1 o6 v: uCalculate the percentage of aluminium oxide (Al2O3) in the sample
" _5 W( j+ K! Vtaken by the formula:
, D' Q3 H' B3 u; D9 Z% K$ k8 s: f3 G% Al2O3 = 100 × (0.005VT)/S
5 a4 T' `& k' r! Ewhere4 Z+ k% G- l1 q" K/ \/ V
V is the number of ml of 0.01 N zinc sulfate consumed in
) P' p: l; i7 V1 ^7 g/ bthe second titration,
* P9 Q8 d0 | p: C3 {) S) ~T is the titre of the zinc sulfate solution,# R: u7 T5 z! g7 L
S is the mass (g) of the sample taken, and
7 _: b& U! H! P+ `( f0.005 = 500 ml / (1000mg/g × 100 ml).
$ W8 P( u9 c3 _# i- n0 u! ESilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
& L+ Q U2 K4 e, z2 jglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
8 ]8 a L* M& s/ R4 q# B( THeat gently over a Meeker burner, while swirling the flask, until- R" O$ [3 J- ~# s8 {) X
decomposition and fusion are complete and the melt is clear, except: f$ w! C0 Q* Z$ f& Z
for the silica content, and then cool. (Caution: Do not overheat the
% }$ T. s+ n) p0 x" Z# A* t, D" rcontents of the flask at the beginning, and heat cautiously during7 L4 V$ C% B& Q9 g' h
fusion to avoid spattering.)! e' [: k% K( R: T' V7 O
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
6 {5 V& R8 L# O& Q7 x6 ucarefully and slowly until the melt is dissolved. Cool, and carefully add" y1 G# W4 x' {" k0 j* B
150 ml of water by pouring very small portions down the sides of the0 t# K0 B N1 R
flask, with frequent swirling to avoid over-heating and spattering. Allow( y% k/ s. w0 X7 H" M
the contents of the flask to cool, and filter through fine ashless filter
9 L! V7 V" J8 o0 Fpaper, using a 60 degree gravity funnel. Rinse out all the silica from/ A# i1 Z& g2 S5 X. z/ x
the flask onto the filter paper with sulfuric acid solution (1 in 10).
; ]1 u+ n; `6 i$ W' s! I8 l( hTransfer the filter paper and its contents into a platinum crucible, dry in
4 l4 f3 I4 R( ]! u; k% }3 t$ z$ {- zan oven at 1200, and heat the partly covered crucible over a Bunsen
/ Q6 y5 s# X! m5 wburner. To prevent flaming of the filter paper, first heat the cover from+ Z3 q5 e% v( G1 ^, L. W2 A
above, and then the crucible from below.
5 T2 y: M' R2 x; `' YWhen the filter paper is consumed, transfer the crucible to a muffle; G2 v( X5 @2 Q z! M3 W+ ?
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
+ K/ J3 r2 R: ?: _weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
) Z/ p5 }# E/ H! fhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
( u+ ^$ A" T4 ?" J0 y$ Von a low-heat hot plate (to remove the HF) and then over a Bunsen
: u+ _9 U5 A1 x6 I; S# b- sburner (to remove the H2SO4). Take precautions to avoid spattering,; l$ b; v n9 ~! o7 i! N8 J4 N0 f
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
' M1 v4 }1 f s3 U3 ]9 Ldesiccator, and weigh again. Record the difference between the two
; i' W6 H' I" \1 w; x+ [! J% o8 |+ U) Kweights as the content of SiO2 in the sample.& }: c! K7 ~$ r( l% t
METHOD OF ASSAY! [% o0 Z% W% K
Accurately weigh about 150 mg of the sample, previously dried at 105o) B( E( a7 |: X
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water; p$ U, @, K3 f; C# {: h
and shake until a homogeneous, milky suspension is obtained. Add 30
( D4 D) `5 \+ V G0 s! zml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially- u% Z, @% ?7 j0 v+ b( ~! U6 x
heat gently, then heat strongly until a clear solution is obtained. Cool,3 O9 m" K/ T3 X, t& z/ Q
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric* ?4 [' o8 F9 \$ w
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
: |3 u. ^: \. Urubber stopper fitted with a U-shaped glass tube while immersing the
& }. a6 j( U6 ]% @; d% ?6 P, Oother end of the U-tube into a saturated solution of sodium
% |0 V. r. L; u& {, wbicarbonate contained in a 500-ml wide-mouth bottle, and generate4 M9 R( q- M6 h" J+ j& r
hydrogen. Allow to stand for a few minutes after the aluminium metal k0 T" `; t$ S) Z1 t) k
has dissolved completely to produce a transparent purple solution.
, X _: R. k, h; HCool to below 50o in running water, and remove the rubber stopper
9 ^. N$ q* G# @! g7 e; i& jcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate# X' ?! v' g8 f! B
solution as an indicator, and immediately titrate with 0.2 N ferric
5 q% T9 N& z) p O/ p$ @% z+ Jammonium sulfate until a faint brown colour that persists for 309 S) e% x* n; A, e1 N4 Q8 x B/ W6 t
seconds is obtained. Perform a blank determination and make any6 Q( g5 o6 e$ s/ a( y
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
8 q9 }4 u$ ?5 uequivalent to 7.990 mg of TiO2.
2 M% `5 Z% {: p$ P4 e |
|