|
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)' y& F( [* E8 a0 V# o. v
; n( i0 | `) Q# Q! G; b0 xJECFA关于二氧化钛(钛白粉)的结论
. k8 s7 ^( u6 v- w X( F" l" ~- ?' k
摘要: 2006年JECFA关于二氧化钛的结论
2 I j% e; J5 SADI值:不作限制。6 s) d6 Z/ y& y# `& {; H" X( o
功能:着色剂7 o; ]7 u a8 z! M
5 v( n1 _' C+ b9 o5 d7 j! h% e
TITANIUM DIOXIDE2 B4 z1 Z k/ m4 S6 J1 D8 v3 }6 g
Prepared at the 67th JECFA (2006) and published in FAO JECFA
- y5 D! \( u* z3 Z) a# ]5 y1 a4 XMonographs 3 (2006), superseding specifications prepared at the 63rd
5 v; ~7 k% q* a7 WJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
3 F3 \7 T( R' n1 w$ P! }Combined Compendium of Food Additive Specifications, FAO JECFA1 j& D5 z X* b- e+ I
Monographs 1 (2005). An ADI “not limited” was established at the 13th ?+ c$ _* e! e, b) p/ c8 A9 _ P
JECFA (1969).) Q6 @5 L Z: H! Z Y; o
SYNONYMS# P! Y: X3 f/ }" g3 S# _
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1718 e' H4 t$ J' w: C) m4 r9 |
DEFINITION
& k# q3 f# P1 q' }( rTitanium dioxide is produced by either the sulfate or the chloride
% N) G' w1 J" j% [process. Processing conditions determine the form (anatase or rutile
) b) t* z/ U3 h. b6 U6 f, Tstructure) of the final product.6 v1 c; v6 K, V1 f ]9 q
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
7 D( n. ]7 k; A. V2 `" ^or ilmenite and titanium slag. After a series of purification steps, the" c* K, Z4 E" e+ O) `8 R
isolated titanium dioxide is finally washed with water, calcined, and. h, z+ O' r# V4 Y1 ^ s: {' V
micronized.: B2 r0 A8 q& b* P6 t, s
In the chloride process, chlorine gas is reacted with a titaniumcontaining
' T8 c0 P1 Y) n8 X! Smineral under reducing conditions to form anhydrous
: D3 \" Q. r) k# J2 ~: }' ]titanium tetrachloride, which is subsequently purified and converted to# B( B; ?/ z& q2 b0 e; W2 q
titanium dioxide either by direct thermal oxidation or by reaction with
$ O3 Q0 ~' v- L6 V8 ]( T: xsteam in the vapour phase. Alternatively, concentrated hydrochloric8 w' e/ V( o* n# a
acid can be reacted with the titanium-containing mineral to form a6 q' R9 c' N2 [4 `
solution of titanium tetrachloride, which is then further purified and0 E8 L- o$ G% Q" V/ F4 a
converted to titanium dioxide by hydrolysis. The titanium dioxide is
/ Y7 y( Y Z/ U- u! zfiltered, washed, and calcined.! {+ x& S# j+ q" Y
Commercial titanium dioxide may be coated with small amounts of
0 s. b: m$ m. j4 N9 oalumina and/or silica to improve the technological properties of the! i6 o, _& @, M7 ], t
product.$ U5 Y& u! ]2 c
C.A.S. number 13463-67-7
" l6 f6 d0 H( V7 S, k- _Chemical formula TiO2
! F' H3 R/ G# W, H+ W1 T5 [; IFormula weight, G' A( d7 d! k5 |0 h* u9 z, |" [
79.88+ `9 e4 W$ g; J9 k0 ~7 K
Assay
: v2 A/ V6 g2 x3 x( wNot less than 99.0% on the dried basis (on an aluminium oxide and
' x8 x( X9 ^* f' Q# R- N* Rsilicon dioxide-free basis)2 r" o- L" G- K
DESCRIPTION4 K, I& D9 \3 E* Y
White to slightly coloured powder
, ^" l2 D0 H: S) R2 Z; a4 ]FUNCTIONAL USES
- H7 T2 q2 ^; T- j( Q* y; BColour
& e9 Z0 b: r- r ?CHARACTERISTICS! _! J4 {: \# |) e0 Q+ K- R; [. B6 |
IDENTIFICATION
6 g3 _6 `( D3 a8 v+ ySolubility (Vol. 4)
+ H1 u$ \2 D- [Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic$ z) t0 ?3 G# ~
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
9 p& e. }, }8 B' msulfuric acid.) O) o4 c4 x. n
Colour reaction9 T6 Y8 K" e7 m1 l, Z( s
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
5 E: L6 C9 k Q8 c" zsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
# _0 F1 d; L; _! a( F7 zwater and filter. To 5 ml of this clear filtrate, add a few drops of+ |0 O) V9 y6 A( q. l/ S
hydrogen peroxide; an orange-red colour appears immediately.
; t6 v }8 F. L' {5 vPURITY" b$ X' s8 a2 E5 r% B
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
7 b& N1 R; c3 i1 ]Loss on ignition (Vol. 4)
' M0 B, Z% {( O' g5 ^9 J( L% nNot more than 1.0% (800o) on the dried basis: s$ I& p& B3 N7 k* V* `) O
Aluminium oxide and/or
1 w5 H5 s+ }+ F, D# f* ~silicon dioxide+ ]- r1 ~" h% r7 m2 _
Not more than 2%, either singly or combined
" Y% K$ N6 _1 p7 T5 J' l" nSee descriptions under TESTS4 K5 ^ p- p1 w8 C3 g' u: l
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
9 D2 Y6 \2 f0 Z. O. valumina or silica.
6 m m. f+ R8 |9 TSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
3 z3 S% M) M3 `place on a steam bath for 30 min with occasional stirring. Filter3 `$ a: t' s f& G' a7 y
through a Gooch crucible fitted with a glass fibre filter paper. Wash8 N9 H9 g; i7 I( p
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the o( G) k( \/ J' l2 G) h
combined filtrate and washings to dryness, and ignite at a dull red5 m' [8 z, C; w; h: { V8 z& u/ q: h& u
heat to constant weight.
! m) ?6 _9 f$ \( o% g) aWater-soluble matter" }, D/ u0 F& I4 \, d9 G) Y# C
(Vol. 4)9 V9 o$ E# U; k2 p m# W
Not more than 0.5%
9 H, H- G. Y6 v0 }Proceed as directed under acid-soluble substances (above), using
4 y! z' j: F6 E$ K/ Cwater in place of 0.5 N hydrochloric acid.
# d5 T6 g0 |5 h0 }, pImpurities soluble in 0.5 N
: Y1 J5 Z; }( ^: S0 whydrochloric acid
* r, Q8 e3 R; w, B; U# \Antimony Not more than 2 mg/kg/ `" d- R5 I- R9 T$ X) _9 F) {
See description under TESTS
( a/ V9 R; Q1 K( ZArsenic Not more than 1 mg/kg) [; S% u) a0 V" @* M: _: u
See description under TESTS
" r+ e" n/ B" h" E0 N! Z8 ?Cadmium Not more than 1 mg/kg
' b$ U% b7 b6 a; W! BSee description under TESTS" E4 D& a: A" A- b! Y7 b+ n
Lead
4 y* @: `. C9 i% ]( LNot more than 10 mg/kg
* c2 \+ P# o. f' k4 o. ~) ^5 MSee description under TESTS# V4 f% w" m4 X- E& {) j- T
Mercury (Vol. 4) Not more than 1 mg/kg
* @3 H/ x& _* U& A. ~Determine using the cold vapour atomic absorption technique. Select a
" o* u6 `' `% t% @, Esample size appropriate to the specified level
- o4 J1 s6 g' h' k* {TESTS
) `1 [2 K! k A1 b: \PURITY TESTS# d5 I A# }8 r) v2 L
Impurities soluble in 0.5 N
$ @" p ?$ p' d8 [3 |hydrochloric acid* p) U* Y+ b; L8 X. h
Antimony, arsenic,0 F$ H1 q' O9 W( H0 t3 O
cadmium and lead, W( V, |5 A8 H# y. P
(Vol.4)
: K, y. c4 m7 A1 u }8 [* K( {Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N" d+ D% e, J/ e* P
hydrochloric acid, cover with a watch glass, and heat to boiling on a: d9 t W; ?. j) m9 Q$ I+ }, z. Z
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml9 _5 E O6 r# H Z% F5 b
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved5 k$ H, J) h; X) J* w
material settles. Decant the supernatant extract through a Whatman
9 o) V; F, @# }! y1 t% kNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
+ Z$ B1 r/ E8 N q. Q8 N' A7 _volumetric flask and retaining as much as possible of the undissolved9 J% g6 r9 T7 Y6 R, y- W# [
material in the centrifuge bottle. Add 10 ml of hot water to the original
' {# |' @+ c. |+ N# y. D6 B- gbeaker, washing off the watch glass with the water, and pour the
0 t/ e% W2 i2 c* qcontents into the centrifuge bottle. Form a slurry, using a glass stirring
" i) P% b, S9 X4 Erod, and centrifuge. Decant through the same filter paper, and collect- S* g; |8 ~6 o
the washings in the volumetric flask containing the initial extract.5 l. v; x8 J( [. G- e
Repeat the entire washing process two more times. Finally, wash the% x$ ^ _# m# E: G% G
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask3 w4 d$ ^* P, E, P a
to room temperature, dilute to volume with water, and mix.
: o, d) U9 l7 {( f* E+ zDetermine antimony, cadmium, and lead using an AAS/ICP-AES
0 t3 @; t0 {; o, d; utechnique appropriate to the specified level. Determine arsenic using the
$ D% h) r4 J k2 p+ S# GICP-AES/AAS-hydride technique. Alternatively, determine arsenic using3 y& T* y: O$ Z& O2 R
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
' K$ h% S5 {. I- K {* p4 n1 g. The selection of sample size and method of sample preparation" h5 D* C5 M) O
may be based on the principles of the methods described in Volume 4.- X. T2 S: h2 X. m5 Y8 p
Aluminium oxide Reagents and sample solutions
9 ?. c/ o; q* p6 b- `% P0.01 N Zinc Sulfate
6 `/ j; G5 h$ VDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to1 o4 r& G k6 z7 A
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
" X. a$ l; E' {* Q" p5 H9 Yof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
1 \/ A3 o& G7 |( j4 J6 kconcentrated hydrochloric acid, heating gently to effect solution, then
- F; E; g. M2 e# h4 ytransfer the solution into a 1000-ml volumetric flask, dilute to volume
' d* P5 J9 c, o5 S9 Rwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
' }5 @! }6 q: n$ O8 `8 W* d }% Rml Erlenmeyer flask containing 90 ml of water and 3 ml of0 w" C: X. S6 A/ g# @2 l
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
) F% C3 |0 {, T; g7 {+ A S% Z25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
* f! V; H8 [8 @: adropwise, ammonia solution (1 in 5) until the colour is just completely
@( ?0 \8 O& _4 Hchanged from red to orange-yellow. Then, add:
4 g% n* k, ^" z& I }1 T7 m& a! y(a): 10 ml of ammonium acetate buffer solution (77 g of# b2 q/ k+ [9 k% F- y; u6 ^0 L
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
2 X* F- m( q+ g. [9 E1000 ml with water) and& n5 F2 O! n) `
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
* d( e8 {( H( y |% x6 U+ k7 zof diammonium hydrogen phosphate in 700 ml of water,; M) Q' q; v3 Q$ \3 l) A
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
5 u. u. J& D, d8 ~ d5 q. f0 Gthen dilute to 1000 ml with water).
' P& Y5 T/ M- r3 j6 p+ E: w' s1 rBoil the solution for 5 min, cool it quickly to room temperature in a3 R# g0 n, F v6 ?6 L s
stream of running water, add 3 drops of xylenol orange TS, and mix." `: x) X6 j% o5 f
Using the zinc sulfate solution as titrant, titrate the solution to the first
0 T+ M" o* y3 pyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
# q7 v0 k" {2 u( S% b7 y6 M- U5 GThis titration should be performed quickly near the end-point by. y- W$ v7 z6 y* e
adding rapidly 0.2 ml increments of the titrant until the first colour& X- p/ U. V1 H0 K8 s
change occurs; although the colour will fade in 5-10 sec, it is the true& w9 r7 v9 O- r( Z" [
end-point. Failure to observe the first colour change will result in an
5 d1 i$ k, m# w( `incorrect titration. The fading end-point does not occur at the second
& k% @5 k3 h; }& G& zend-point.): y1 l) `3 m: B6 ^, k. I4 Q
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
/ k7 R# B5 _/ m6 v7 B+ ^stream of running water. Titrate this solution, using the zinc sulfate
9 }0 x# G- N( f+ A! ~4 c6 J) esolution as titrant, to the same fugitive yellow-brown or pink end-point
# z8 K) o7 r. Y+ q& A) \$ _, Xas described above.4 M0 n0 Y7 ]4 P& |* x( J
Calculate the titre T of zinc sulfate solution by the formula:5 v i' y3 r( x) H9 j* K: G
T = 18.896 W / V
6 c, ~- V9 s9 B1 ~. c3 @2 Lwhere5 L1 S3 ~ d7 f6 W# |( i# u1 J
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution7 K! p) d5 d4 X' U
W is the mass (g) of aluminium wire
2 j3 q& ^5 O+ q- u. Z9 H# m; pV is the ml of the zinc sulfate solution consumed in the) P, Z" D6 ^7 M2 i
second titration
# L6 D+ i, z: ]. f9 i" ]) h- }18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
' r& q# k3 R [ z0 L5 XR is the ratio of the formula weight of aluminium oxide to
* @ v Q" L* J0 ]. r7 J$ Ithat of elemental aluminium.
# j- P# f+ D( s3 a/ U. h8 WSample Solution A4 J3 F4 k# V k& _! v
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
, ~6 X& ?9 K: V! l% ^: D N/ mglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
, t, u% |1 y7 x5 m/ f(Note: Do not use more sodium bisulfate than specified, as an excess
: s0 p d/ q/ ?) F' D7 Cconcentration of salt will interfere with the EDTA titration later on in the
$ Y+ N7 V; r9 Y0 A6 P7 n1 d0 Rprocedure.) Begin heating the flask at low heat on a hot plate, and% P4 [" E5 ~0 [2 z2 V1 s
then gradually raise the temperature until full heat is reached.
& Y! Q% X3 s# P% A4 x: e: L: u8 Z$ s! _(Caution: perform this procedure in a well ventilated area. ) When
. b/ P& M z9 J' \spattering has stopped and light fumes of SO3 appear, heat in the full
/ o8 ^4 h$ V2 L, I, p A$ A% |flame of a Meeker burner, with the flask tilted so that the fusion of the6 ? |' c% l, w' l4 V8 z
sample and sodium bisulfate is concentrated at one end of the flask.' \/ ~1 m7 G% [* }! |* y% e8 y
Swirl constantly until the melt is clear (except for silica content), but
* P! Y \4 Y8 Wguard against prolonged heating to avoid precipitation of titanium
1 L( `/ f% a/ ~7 h3 [( e( ]! S9 Edioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until0 G/ x1 p# ?5 S) v
the mass has dissolved and a clear solution results. Cool, and dilute to
" d. r; `7 x- k# z2 n120 ml with water. Introduce a magnetic stir bar into the flask.
. }1 z; l0 n4 t3 _* r I+ g! PSample Solution B
7 A6 `6 G( C# bPrepare 200 ml of an approximately 6.25 M solution of sodium$ s9 ~% ]: Z1 _1 Z0 C
hydroxide. Add 65 ml of this solution to Sample Solution A, while$ m8 y& [* M; I: i+ R
stirring with the magnetic stirrer; pour the remaining 135 ml of the
5 u2 S+ n% Q/ t Q! h7 m+ z4 Oalkali solution into a 500-ml volumetric flask.
" B. l: |' }* t VSlowly, with constant stirring, add the sample mixture to the alkali9 N' Z Y! [# `- X* X
solution in the 500-ml volumetric flask; dilute to volume with water,
' a7 t( H6 R7 ^+ zand mix. (Note: If the procedure is delayed at this point for more than/ z$ Q8 N. W! t) x8 P- e* u/ [
2 hours, store the contents of the volumetric flask in a polyethylene% J. ^0 [. g2 |% |
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
4 X6 H3 {$ `! Ythen filter the supernatant liquid through a very fine filter paper. Label
1 p* k& [6 m( i- W+ othe filtrate Sample Solution B.
* W6 _8 O2 L. p2 P" @: R' dSample Solution C
& i$ B( j$ \1 LTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer# h4 _ j) T, w& }5 }5 D# S: E! e7 J: K
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid! y) ^: x% t- t
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
2 a- q6 T* t" ?3 @( k) f/ A3 BM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
: u- Z) J+ [% i& q ~; Dknown, calculate the optimum volume of EDTA solution to be added
2 k9 q; l |3 N9 A1 M3 Vby the formula: (4 x % Al2O3) + 5.]- w% c& j% ]2 m y1 g( i
Add, dropwise, ammonia solution (1 in 5) until the colour is just
' T8 S: S5 B6 H$ M; ~4 n5 e0 _completely changed from red to orange-yellow. Then add10 ml each* W2 m* ?: N* \
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
* k6 o# z4 @" i+ Rroom temperature in a stream of running water, add 3 drops of xylenol/ S: W# d2 O, F4 Y& a9 [! t8 E
orange TS, and mix. If the solution is purple, yellow-brown, or pink,& h: E" N+ o1 i- j' R, {1 E
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired9 W% U" Q: B* Z
pH, a pink colour indicates that not enough of the EDTA solution has
2 }4 b, z1 Z% _5 x9 `- Sbeen added, in which case, discard the solution and repeat this7 j d; R: B) f& S8 x6 f8 x
procedure with another 100 ml of Sample Solution B, using 50 ml,
9 G) i$ X4 x& z% ^) L5 u& i4 F! e' E# rrather than 25 ml, of 0.02 M disodium EDTA.
# u; J, }1 h( k; VProcedure" `1 s: }# ]( {5 C+ y
Using the standardized zinc sulfate solution as titrant, titrate Sample
' G/ `2 {- F3 D0 I xSolution C to the first yellow-brown or pink end-point that persists for
. I( T9 `3 ^1 }: l; X5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
& N, Q- b( W3 U+ b; d" g- F3 Htitration should require more than 8 ml of titrant, but for more accurate
2 z% o- z! D' G6 U* ^1 _work a titration of 10-15 ml is desirable.& Z& e2 t; Q" U. t
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5& V/ t* s' o+ n1 d
min, and cool in a stream of running water. Titrate this solution, using
" F( D+ ` b% t: w" i7 }the standardized zinc sulfate solution as titrant, to the same fugitive
4 R1 x: I3 I7 y- iyellow-brown or pink end-point as described above.: h8 [ y- u3 V
Calculation:
5 Q1 s3 x1 o2 C/ Z& fCalculate the percentage of aluminium oxide (Al2O3) in the sample
- b+ J) ^& s+ V0 _8 b3 \taken by the formula:
) v# f; b0 o; w3 x% Al2O3 = 100 × (0.005VT)/S5 |4 s9 a9 Y! d9 j# {" v8 Y5 h% s
where0 ?$ ~6 m, ]& V- e+ _
V is the number of ml of 0.01 N zinc sulfate consumed in+ O" s5 q/ |' S
the second titration,4 o% D% D8 Q% T3 v
T is the titre of the zinc sulfate solution,- n. G6 _% D( _; e
S is the mass (g) of the sample taken, and
$ l2 M( q+ B4 s0.005 = 500 ml / (1000mg/g × 100 ml).6 \" b. ^6 t) ^" X: K+ H, U2 ]# t
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
6 n: D D$ d) R2 Iglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
6 ]2 L6 L+ o5 w/ w( V B+ C, d1 lHeat gently over a Meeker burner, while swirling the flask, until
% }6 o/ d5 m6 C- }decomposition and fusion are complete and the melt is clear, except' m4 J. | w4 Y6 R* H F
for the silica content, and then cool. (Caution: Do not overheat the
5 ` k' B9 v& Ccontents of the flask at the beginning, and heat cautiously during
5 x' P2 l7 Z' sfusion to avoid spattering.)
- C$ ]0 f7 M& k8 [1 w. N8 z$ ATo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat' _+ d8 S5 I* H
carefully and slowly until the melt is dissolved. Cool, and carefully add
8 a9 g! `# u6 a% A( _* U150 ml of water by pouring very small portions down the sides of the
, J3 ?$ R- P$ a7 H: f3 Hflask, with frequent swirling to avoid over-heating and spattering. Allow
0 ?9 w5 ~: ^8 }- a5 e+ zthe contents of the flask to cool, and filter through fine ashless filter
7 K" E( t. }, _) \+ b+ G* upaper, using a 60 degree gravity funnel. Rinse out all the silica from
# H, e+ D, T3 Z( Lthe flask onto the filter paper with sulfuric acid solution (1 in 10).5 ^& b$ u' w3 U1 ^. q0 h- Y
Transfer the filter paper and its contents into a platinum crucible, dry in9 F W/ _ u/ |, y/ c) s
an oven at 1200, and heat the partly covered crucible over a Bunsen
' J" q9 `- h$ v, T: C2 J$ g# n! zburner. To prevent flaming of the filter paper, first heat the cover from }) R/ J- J( s+ A5 Z& r
above, and then the crucible from below.2 W# _0 Z( v1 K" Z, n
When the filter paper is consumed, transfer the crucible to a muffle8 {; Y0 E7 _+ f6 a; r1 w! P2 e, m8 s! G
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
3 D0 m. Z1 e4 z4 t6 ?- U! C1 Lweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
8 l: a' c& R1 J* J; N+ O. yhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
% S0 G% H; l, y2 `# M6 aon a low-heat hot plate (to remove the HF) and then over a Bunsen
0 w* R- c5 U) ^" e; iburner (to remove the H2SO4). Take precautions to avoid spattering,
; w( v5 A, @7 x( _especially after removal of the HF. Ignite at 1000o for 10 min, cool in a N' Q8 D" n7 |8 r
desiccator, and weigh again. Record the difference between the two
' W" `, Y6 e7 ?" w% U) o) ?weights as the content of SiO2 in the sample.
: F: D: L8 O3 k) D; lMETHOD OF ASSAY
: h8 ~1 @0 Q/ a1 ]Accurately weigh about 150 mg of the sample, previously dried at 105o
& I" b7 @1 f' Z6 l; A. d# Mfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
) @7 p) J9 y/ m' j5 jand shake until a homogeneous, milky suspension is obtained. Add 30
' x; }3 T2 P* \) ^ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially$ {5 X, |" b4 ~8 B" U5 y5 J
heat gently, then heat strongly until a clear solution is obtained. Cool,; V8 B ]7 u, R$ ]& _9 h. Z0 x/ w
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric$ I& P, u$ u+ ]& b1 q: a" {
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
! g: J: x2 X) u) wrubber stopper fitted with a U-shaped glass tube while immersing the. n f& @% `* {: ~; z
other end of the U-tube into a saturated solution of sodium+ ]2 n6 P+ ~* m1 t, n7 r
bicarbonate contained in a 500-ml wide-mouth bottle, and generate* Z0 G2 G9 I5 }. ]
hydrogen. Allow to stand for a few minutes after the aluminium metal! c8 q- q5 M' J/ J& X
has dissolved completely to produce a transparent purple solution.
2 I5 }3 B9 s2 ~# kCool to below 50o in running water, and remove the rubber stopper3 G6 G/ D9 P) @! P& M0 T+ _& ]& h
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
x) H2 l/ E5 O; ^solution as an indicator, and immediately titrate with 0.2 N ferric( k# R- S. @7 l8 l( z2 V# |6 d# `
ammonium sulfate until a faint brown colour that persists for 30
- L4 [, b4 M4 a6 K' ]% u- Gseconds is obtained. Perform a blank determination and make any
( ~ ]" M3 S2 \ j% Dnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is. @4 e- m i& P: o' w
equivalent to 7.990 mg of TiO2.
, [4 H% o) C" s, r7 R: O0 X4 l |
|