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二氧化钛(钛白粉)
二氧化钛(钛白粉)1 v" I3 B! q' X2 O9 Q
; [! l6 Y) T! |, `
JECFA关于二氧化钛(钛白粉)的结论
- F9 i. ]" Y2 w1 h( Q' @) H# f5 t5 x
. [6 S5 k6 ]' i8 Q摘要: 2006年JECFA关于二氧化钛的结论
. z/ G& x! W7 N/ y/ Z7 M2 n f4 KADI值:不作限制。
3 K5 F9 \( O1 F功能:着色剂
# ^6 Y: K( m! V* Z/ G4 g4 E1 C' |" k: H0 M+ W
TITANIUM DIOXIDE
8 I" z' C# n" x! a7 f; d7 v3 HPrepared at the 67th JECFA (2006) and published in FAO JECFA
- n# l5 W T: {0 z5 z4 m) y" SMonographs 3 (2006), superseding specifications prepared at the 63rd- ` w' E: j5 Y
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
4 B( W6 @9 x) B5 n( sCombined Compendium of Food Additive Specifications, FAO JECFA
& |3 z$ R9 x3 b$ ~* zMonographs 1 (2005). An ADI “not limited” was established at the 13th* Q8 j# d0 g# X3 [1 J" w
JECFA (1969).
- J7 |4 y8 V: b1 DSYNONYMS
" P9 s! j6 h8 s' `4 z! A( O9 M5 ZTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
' K/ S# C G$ Z7 s1 l: rDEFINITION
4 z! o) ]: C5 _+ ?: t' ?5 b$ pTitanium dioxide is produced by either the sulfate or the chloride
, P# B) `; F- ?% zprocess. Processing conditions determine the form (anatase or rutile" h: J; t8 \) B2 [+ g- ]9 }( j" ]
structure) of the final product.
7 w! r2 D: V5 j; MIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
7 j6 }* w5 n$ `% W& j( {6 P, v& Bor ilmenite and titanium slag. After a series of purification steps, the% i' f- @' u8 b* V4 M
isolated titanium dioxide is finally washed with water, calcined, and! Z& ^% r2 r# S# P: D# G/ T- Z; Y
micronized.6 ]- ]+ O+ \/ L" v
In the chloride process, chlorine gas is reacted with a titaniumcontaining/ s$ O6 r' _; O/ w; S' _/ q
mineral under reducing conditions to form anhydrous+ f3 {6 y+ Z+ d' p: {; n/ b
titanium tetrachloride, which is subsequently purified and converted to
M+ E) @; y/ Q- O$ qtitanium dioxide either by direct thermal oxidation or by reaction with
2 d. j7 _4 d W+ d+ `* [1 Y1 Ksteam in the vapour phase. Alternatively, concentrated hydrochloric
5 t7 w l: w; U- B+ b( V! Dacid can be reacted with the titanium-containing mineral to form a& p7 x0 D) b5 A7 ]5 J5 {
solution of titanium tetrachloride, which is then further purified and
# a' d+ d2 H7 i9 Pconverted to titanium dioxide by hydrolysis. The titanium dioxide is
, I( P# [+ {6 x0 ^( ]filtered, washed, and calcined.. J% i; D: g1 p5 M1 X5 m
Commercial titanium dioxide may be coated with small amounts of
/ m p7 Z5 a. malumina and/or silica to improve the technological properties of the
7 j* j. d$ z" C. H! Nproduct.
' J! G) c8 H/ uC.A.S. number 13463-67-7( \* Q: q% l' T6 Y4 @# e0 l2 p' g
Chemical formula TiO2
8 t, J3 _, r' aFormula weight
! [' K) T/ Z- ?" j: X* Z" S79.88
+ L. j: n8 Y8 p$ cAssay6 N5 o& m" c8 R! z q& O6 q
Not less than 99.0% on the dried basis (on an aluminium oxide and( R/ P: u. ]* Y. h @2 H `
silicon dioxide-free basis)
7 k _/ Q2 b3 @* pDESCRIPTION
$ ~( E/ q4 U* A2 RWhite to slightly coloured powder( c& h. V+ o5 v* j
FUNCTIONAL USES c6 q) @& J7 ]4 M( i
Colour' C. Y! Y" _3 h, K
CHARACTERISTICS
) {2 t- N; l( ?9 a+ BIDENTIFICATION( O. ~3 ^; x1 n7 v' p" r" l
Solubility (Vol. 4) j8 P( H+ }' y
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
3 |9 H6 P% a( x1 ^$ j+ ]solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
$ [4 F0 A+ F3 U- c$ Msulfuric acid.
4 E3 |$ G$ J2 nColour reaction$ C2 h) x% F! |$ s: \8 r
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
+ H7 X% D |; T3 I, o5 {% hsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with4 ]. ], t- g, o4 m6 ]/ c, t# t
water and filter. To 5 ml of this clear filtrate, add a few drops of
0 F! z3 }1 @: o% [0 f+ h/ ghydrogen peroxide; an orange-red colour appears immediately.& w1 ^8 |) j+ W! ]
PURITY
: Y7 |: l$ T. F5 h/ vLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
; A' l& ^ Q/ U0 j8 _* W5 {1 ILoss on ignition (Vol. 4)
. i: j; z4 Q3 {' {5 X" ~: `. NNot more than 1.0% (800o) on the dried basis
0 t2 t' X1 B5 uAluminium oxide and/or
$ {. r6 v9 p2 `5 z: Xsilicon dioxide$ ]; p+ v$ \" W& `0 a6 E$ C
Not more than 2%, either singly or combined6 U$ G. Y' k4 L# v" T+ m3 j& H
See descriptions under TESTS: K! N) Q8 u7 S; G( R' k h
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing" t. h, Y/ B/ C
alumina or silica.5 s. \2 p7 V5 H
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
0 ^9 O7 f* G2 l& L" d1 cplace on a steam bath for 30 min with occasional stirring. Filter
% J: ?; `1 w# p4 Pthrough a Gooch crucible fitted with a glass fibre filter paper. Wash0 M1 r5 {7 u( a4 M4 ]' v/ N
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the b+ Q; w8 _! s2 o9 @3 `% q. O
combined filtrate and washings to dryness, and ignite at a dull red
" {) |9 u) {0 _/ U& Kheat to constant weight.
* q& j2 v0 `; h+ U- T( n! UWater-soluble matter* @8 n0 O7 v- [. y" `
(Vol. 4)$ m$ j* p8 I! M! J
Not more than 0.5%- w1 `- _ J" C- a5 m
Proceed as directed under acid-soluble substances (above), using
6 K9 D; o, g i: l5 K5 w, L }water in place of 0.5 N hydrochloric acid.: r& Y! u, M' {9 H7 d- H
Impurities soluble in 0.5 N |* s9 p" e$ I6 u$ |: J: I2 n
hydrochloric acid- P. w$ ~, V4 A: s- B% F" X$ Z
Antimony Not more than 2 mg/kg
( f$ J, k9 T: j. G. Q' {) \See description under TESTS
# M3 j" R, U# \ I$ d9 S d1 F0 A% uArsenic Not more than 1 mg/kg
1 J( M, E7 L' V- a/ L' E0 PSee description under TESTS
0 D% Q* f4 `- V, a O( \8 XCadmium Not more than 1 mg/kg* j! L% x# O( O' M; H
See description under TESTS8 P) e; [6 n: t% T
Lead
: E) X+ ?' ]2 S0 p: O/ GNot more than 10 mg/kg
' H/ i6 S3 N* i& _9 E0 a" SSee description under TESTS# p* e( ?2 a. l
Mercury (Vol. 4) Not more than 1 mg/kg3 Y5 Z, r, a) I. H2 a+ X* }
Determine using the cold vapour atomic absorption technique. Select a9 Y" S7 Q4 E0 _) q4 K
sample size appropriate to the specified level
0 j: `7 _! J; D4 E; ], D" H$ BTESTS: H3 V: z* i0 J i9 D/ J6 L: s2 B
PURITY TESTS6 A! w+ R! g0 T& U% D f; m
Impurities soluble in 0.5 N
: A2 X" w! F7 y, mhydrochloric acid. M5 z( m4 C( I0 K ~0 o
Antimony, arsenic,8 p4 g; p8 w3 X" M! [
cadmium and lead
5 b0 E2 g1 S7 g/ A(Vol.4)* C; c- p- y' I6 F' l
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N3 N/ d( @1 Z; ~7 p- G3 u
hydrochloric acid, cover with a watch glass, and heat to boiling on a
! O& S. P0 |# g9 m9 k3 K& Khot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml" Y# e8 B* O$ L* x- }
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved% |, _4 h8 ]) y8 ^
material settles. Decant the supernatant extract through a Whatman
* f: D4 u s4 i8 `7 A( `5 G7 ONo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
, U- F3 v0 I3 C' k P8 Yvolumetric flask and retaining as much as possible of the undissolved, t! y0 O/ w z% ?9 r$ k( M
material in the centrifuge bottle. Add 10 ml of hot water to the original
# |' j( ?. B" g, Dbeaker, washing off the watch glass with the water, and pour the5 _# i' ^( g* J! O4 O2 F$ W
contents into the centrifuge bottle. Form a slurry, using a glass stirring3 s. g0 e1 ]6 b, r% d) v
rod, and centrifuge. Decant through the same filter paper, and collect
9 z* B: j, O- w2 L+ _* \0 [% P/ Ethe washings in the volumetric flask containing the initial extract.
5 E1 ^& R/ B. ^* ` W: GRepeat the entire washing process two more times. Finally, wash the
! K. K: K9 G* g1 v$ Efilter paper with 10 to 15 ml of hot water. Cool the contents of the flask. f, ~' C" T8 H% D3 ]5 \0 @1 I
to room temperature, dilute to volume with water, and mix.( X" C( N1 `, Q0 W6 s
Determine antimony, cadmium, and lead using an AAS/ICP-AES
/ o: ~2 o. T7 n0 Atechnique appropriate to the specified level. Determine arsenic using the
1 k; j# Y- W5 j# k2 x: \ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using( M9 u+ g6 @6 z6 g" |4 y) H; ~
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
y" ~4 l* m* L$ {6 P8 U1 g. The selection of sample size and method of sample preparation
( R$ j/ I3 C `$ S( I0 L2 @7 Lmay be based on the principles of the methods described in Volume 4.
4 ~) v( {" C5 e/ Z& {Aluminium oxide Reagents and sample solutions* i3 K, J5 L; ~2 `2 J, ?6 q
0.01 N Zinc Sulfate
5 ~8 \8 a* O6 G& c9 a$ aDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
6 E$ B4 Q6 Y+ E7 Y2 s6 {6 X+ {make 1000 ml. Standardize the solution as follows: Dissolve 500 mg5 @7 |2 \' e- F E$ l
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of ^% Q! m9 a8 n8 h8 Y n
concentrated hydrochloric acid, heating gently to effect solution, then4 [/ k1 q# |: Z" R- H1 Z& p2 f- e
transfer the solution into a 1000-ml volumetric flask, dilute to volume9 x( J$ ~# D- r1 Z+ ?, M7 N
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5003 a e) R& M# X
ml Erlenmeyer flask containing 90 ml of water and 3 ml of/ F* V* k$ r0 a
concentrated hydrochloric acid, add 1 drop of methyl orange TS and# o8 }0 P r+ e$ _8 J; V, U4 o4 a( o4 x
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
8 E/ y4 D. D. E% m, Xdropwise, ammonia solution (1 in 5) until the colour is just completely
1 N2 S% i' ^# U6 Nchanged from red to orange-yellow. Then, add:
$ G4 _" ^0 X" N9 R6 Q! G(a): 10 ml of ammonium acetate buffer solution (77 g of; J0 @% d- {% w( d/ M
ammonium acetate plus 10 ml of glacial acetic acid, dilute to: |3 B" n# Q6 v5 B! K) p2 x
1000 ml with water) and
& G! F3 c2 _ l+ T. n' X9 {(b): 10 ml of diammonium hydrogen phosphate solution (150 g- I. G( I7 f/ [
of diammonium hydrogen phosphate in 700 ml of water,
4 ]/ E3 I# a- K, w# T1 oadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
0 h2 f7 r8 H) o: t5 Athen dilute to 1000 ml with water).
6 ?$ {1 @4 C5 }5 C; I3 k+ g$ I. ABoil the solution for 5 min, cool it quickly to room temperature in a
9 g& t1 x* D8 F3 e# mstream of running water, add 3 drops of xylenol orange TS, and mix.% R9 y# T% Y1 s4 n) L+ l8 u
Using the zinc sulfate solution as titrant, titrate the solution to the first
2 d6 d2 g$ F( p7 ^! ^yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:& |7 N- C1 W( }' D1 _
This titration should be performed quickly near the end-point by1 M% W8 B' Y2 p
adding rapidly 0.2 ml increments of the titrant until the first colour& h9 _5 t$ w. g7 I. p {9 N
change occurs; although the colour will fade in 5-10 sec, it is the true# s$ L: @2 {( v7 ~! \4 c9 m. p$ _
end-point. Failure to observe the first colour change will result in an* t4 _ i' @. f
incorrect titration. The fading end-point does not occur at the second% t: e8 z' G, Q. |# h; H2 |
end-point.)
1 g8 p+ ^& | O$ s7 `Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
{6 T* x k5 rstream of running water. Titrate this solution, using the zinc sulfate. {& v( P3 [, n+ B+ Z' t
solution as titrant, to the same fugitive yellow-brown or pink end-point( }; d/ M1 M7 T; L8 ^+ n
as described above.8 H+ P5 n8 o7 b8 }+ S% P7 Z. I' G( r
Calculate the titre T of zinc sulfate solution by the formula:
3 A% @" T/ z4 |T = 18.896 W / V
/ q+ O* V: P; c8 |+ m- M$ rwhere
( ?/ u7 T n% S. G5 C: d( ^T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
/ g- B3 D- x' Q {+ f2 |$ l ?W is the mass (g) of aluminium wire
6 Y3 R" F# I1 T6 \V is the ml of the zinc sulfate solution consumed in the
$ U4 H3 P9 r9 V8 g4 wsecond titration
' n2 D5 K, e l: b; \) e( P18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
1 H; i: ], F* yR is the ratio of the formula weight of aluminium oxide to U: x, I5 E2 [8 T7 Q5 p
that of elemental aluminium.$ x3 A$ V3 C9 H* D9 C
Sample Solution A
+ x7 o/ s( |( [% @Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
! z$ I: E# y0 v. _) U- x+ bglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
* p/ r& A. E) g9 i- w. D(Note: Do not use more sodium bisulfate than specified, as an excess
4 W2 d. ~3 k& p! _. q. `* xconcentration of salt will interfere with the EDTA titration later on in the9 J3 h2 k4 I/ \1 j9 J9 Q/ x0 d( [
procedure.) Begin heating the flask at low heat on a hot plate, and
, v$ e2 O; U7 [: E5 |8 jthen gradually raise the temperature until full heat is reached.0 t& u; [% ], G' s1 }! V
(Caution: perform this procedure in a well ventilated area. ) When. b/ q, a0 {& O0 w& i8 Z' ~
spattering has stopped and light fumes of SO3 appear, heat in the full9 c% c$ {4 e$ ], l: T$ \% A: X
flame of a Meeker burner, with the flask tilted so that the fusion of the
; u! K2 T) S: ]) A( vsample and sodium bisulfate is concentrated at one end of the flask.8 m$ \& S4 l+ O# z0 h! v9 n
Swirl constantly until the melt is clear (except for silica content), but
( U$ B* _7 i- W; E6 h8 f# \guard against prolonged heating to avoid precipitation of titanium
% R" E* Q+ z% {8 j: J5 q9 m7 \dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until4 D: }) w3 q8 W' y7 t1 y' R3 h; C0 @
the mass has dissolved and a clear solution results. Cool, and dilute to; O) x4 y! P* Q d5 r e8 A
120 ml with water. Introduce a magnetic stir bar into the flask.
' r3 W3 X6 Q0 H) ~9 p- QSample Solution B3 J$ c7 z8 L: k8 D' G7 E$ N: H
Prepare 200 ml of an approximately 6.25 M solution of sodium& V9 Q2 G/ N0 C2 F/ k
hydroxide. Add 65 ml of this solution to Sample Solution A, while& U$ }$ G; U7 M' Q/ i
stirring with the magnetic stirrer; pour the remaining 135 ml of the% b1 [" e7 X. ~6 g
alkali solution into a 500-ml volumetric flask.: ~) d$ A, s; v
Slowly, with constant stirring, add the sample mixture to the alkali. w) X" p, ?1 K8 d* c6 G. x
solution in the 500-ml volumetric flask; dilute to volume with water,
, O5 I" z4 Q8 F; G: [$ Nand mix. (Note: If the procedure is delayed at this point for more than
0 F S' ~6 V, q. H* \2 hours, store the contents of the volumetric flask in a polyethylene
& E9 X2 n7 T! |0 dbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),8 N& r% y5 A7 Y8 s; ^/ I
then filter the supernatant liquid through a very fine filter paper. Label
* a2 c+ _ D* `; c/ C! mthe filtrate Sample Solution B.: g9 \( z; B( n2 g/ b( a! n2 @
Sample Solution C& k; N) s2 B \% Q$ {4 s' y2 w6 S* P2 z
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
5 N8 ~( y E8 e% ~ Q: C+ cflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
8 i7 I6 a ]% V! D: @) Tsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02& t# j8 P4 W5 v. @# A- \ K
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
* U+ h" @" g& u: k- t. @3 t5 n* }known, calculate the optimum volume of EDTA solution to be added9 R* ?* d6 u9 Z: `1 ^8 i- K; C
by the formula: (4 x % Al2O3) + 5.]
# g4 D q2 P2 j0 U; r& ?Add, dropwise, ammonia solution (1 in 5) until the colour is just$ F3 N/ Y$ m7 P) T! z5 ~! [
completely changed from red to orange-yellow. Then add10 ml each0 ^# ]" G& Q3 F, e. d$ }2 K7 Y
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to4 l, J& Z$ {( l: r6 Y5 g: ]
room temperature in a stream of running water, add 3 drops of xylenol
: \. {" q7 @ G& a9 ]- q G q! @orange TS, and mix. If the solution is purple, yellow-brown, or pink,
! h8 v5 M0 ?# ]1 W( I/ Fbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired* k8 ?/ m; _$ E% H x$ h. ^! q* A
pH, a pink colour indicates that not enough of the EDTA solution has+ g3 m) Y! X% \
been added, in which case, discard the solution and repeat this3 x+ i: r" @7 ]' T- M' U- R
procedure with another 100 ml of Sample Solution B, using 50 ml,
6 n' k+ M9 ?7 u Grather than 25 ml, of 0.02 M disodium EDTA.
w- b; V- P: K9 N/ VProcedure
# ?# s: z1 P9 L n* ]+ M( SUsing the standardized zinc sulfate solution as titrant, titrate Sample
2 u0 m- m7 |1 `/ p% _( n; ASolution C to the first yellow-brown or pink end-point that persists for
! e# }- z! }1 h k0 i: G5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first7 E) x" }% p# x6 c4 C, V' ^/ z
titration should require more than 8 ml of titrant, but for more accurate
9 ~: t8 T. c6 |7 J1 Wwork a titration of 10-15 ml is desirable.5 Z' X U% W, z+ E [6 t
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
1 Y/ _! l5 J6 X7 R0 R# y3 dmin, and cool in a stream of running water. Titrate this solution, using- b6 J4 d% K! s' G
the standardized zinc sulfate solution as titrant, to the same fugitive
$ ^. ?1 g+ A" K/ j' q* l5 zyellow-brown or pink end-point as described above.
# k5 C6 K z* b) P' T: ^4 gCalculation:6 w5 {0 d3 R. Z' v/ f0 `
Calculate the percentage of aluminium oxide (Al2O3) in the sample
( P0 R2 g1 ~9 O$ _taken by the formula:* l: j# P+ b* V$ z5 A" X
% Al2O3 = 100 × (0.005VT)/S* e! H6 {/ a, Z- G" o! e
where
0 M5 ~6 U- C0 ~( xV is the number of ml of 0.01 N zinc sulfate consumed in
# w; W1 T: h2 O( f( E9 A# tthe second titration,: R- a6 I# z6 B1 V. w( r% a) {0 j
T is the titre of the zinc sulfate solution,/ u. R( Z* e; k, K3 W2 W
S is the mass (g) of the sample taken, and. G" \6 l" I- i5 p# g P/ y4 b; Y z
0.005 = 500 ml / (1000mg/g × 100 ml). ]0 l7 {' [$ C8 C
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
7 q% r! B, }, y- }$ N: }glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).! H+ k2 o5 c# g7 C' ?8 P
Heat gently over a Meeker burner, while swirling the flask, until9 z% E7 u2 Y, O7 f
decomposition and fusion are complete and the melt is clear, except
: K* }1 @8 ^: R: E6 Qfor the silica content, and then cool. (Caution: Do not overheat the$ G2 d- M. ?; ] ^
contents of the flask at the beginning, and heat cautiously during
7 l ]# U8 n# m0 X/ n/ ?fusion to avoid spattering.), h7 K9 F! t6 M; |# s
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
/ S8 h/ ?; @# o& s1 \/ \3 Ycarefully and slowly until the melt is dissolved. Cool, and carefully add
# u# ]2 l+ @, H! f150 ml of water by pouring very small portions down the sides of the3 l+ Q/ ~) o" i1 ~/ _* L
flask, with frequent swirling to avoid over-heating and spattering. Allow. B0 v- z9 w* ^* f \: @: ^1 k& ~
the contents of the flask to cool, and filter through fine ashless filter: ^- |* F0 v5 d9 |, O3 {
paper, using a 60 degree gravity funnel. Rinse out all the silica from, K4 O) b+ w) |/ j+ e% B! ~1 X
the flask onto the filter paper with sulfuric acid solution (1 in 10).
0 Q# `# \# s* r" a6 m8 l" _Transfer the filter paper and its contents into a platinum crucible, dry in
& v& L1 [- {2 x+ f( R% man oven at 1200, and heat the partly covered crucible over a Bunsen
# w, }+ @- [" Q$ @burner. To prevent flaming of the filter paper, first heat the cover from
' `0 c* i5 ?, A4 S3 d" T( babove, and then the crucible from below.; }. K5 Q( r S3 C
When the filter paper is consumed, transfer the crucible to a muffle
* a, ]7 S+ S+ ]: [2 \7 ^furnace and ignite at 1000o for 30 min. Cool in a desiccator, and" O5 o5 B1 X% H5 X
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated: U* O8 J# X5 k% E9 Z* k) I
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first8 b! i# `' E$ [4 [
on a low-heat hot plate (to remove the HF) and then over a Bunsen' h8 x" g, Z9 N5 B1 A
burner (to remove the H2SO4). Take precautions to avoid spattering," P* _! T6 [0 n. k7 G0 ? b
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
3 M# B2 i# n5 K& ?desiccator, and weigh again. Record the difference between the two
5 K& L4 V+ x5 C) \ I6 o, i6 Yweights as the content of SiO2 in the sample.) u( r3 G0 b5 z* O
METHOD OF ASSAY1 A$ t. S0 ? ?4 M( p
Accurately weigh about 150 mg of the sample, previously dried at 105o! j& j- ~) o" ]9 T, |3 V
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water. N7 p: n/ n% a
and shake until a homogeneous, milky suspension is obtained. Add 309 g2 @ C. Z4 G7 t: R! e- v! q5 G
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
* e; \0 x5 Y, P _. Uheat gently, then heat strongly until a clear solution is obtained. Cool,
. ]5 D& C" x6 k2 W/ \' cthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
1 V$ E4 R* `5 O6 R7 Aacid, and stir. Add 3 g of aluminium metal, and immediately insert a# l* J5 U! {: W) x) M5 J7 {$ x
rubber stopper fitted with a U-shaped glass tube while immersing the( ]* A9 e5 o' V, [% A
other end of the U-tube into a saturated solution of sodium2 k& Y9 t; r, Z
bicarbonate contained in a 500-ml wide-mouth bottle, and generate7 `; L% D3 U' `+ A8 ^5 K
hydrogen. Allow to stand for a few minutes after the aluminium metal
: }9 d1 B. ~2 g1 w1 E" Zhas dissolved completely to produce a transparent purple solution.# r; S5 M0 h) N7 x) S; t, h1 v
Cool to below 50o in running water, and remove the rubber stopper
! t; p. h' D% |5 h. i( c, zcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
9 V9 r6 |% H) |; X) |solution as an indicator, and immediately titrate with 0.2 N ferric* R4 I: r' r8 ?: i6 W1 u" X
ammonium sulfate until a faint brown colour that persists for 30; M' N6 h( r" ^% V% M# q
seconds is obtained. Perform a blank determination and make any
X! j. S! x# F/ |2 M/ Nnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
/ [2 f% m! ?6 o8 wequivalent to 7.990 mg of TiO2.
" R- a9 U0 e: r$ r/ N |
|