|
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)+ z6 @* U @: Z7 H
o( M4 L5 a6 ]: P( y
JECFA关于二氧化钛(钛白粉)的结论
1 K+ h; h/ X( E* a, J5 w
3 o- ^. e$ t- L! z! i5 F% J7 G4 l- n摘要: 2006年JECFA关于二氧化钛的结论4 k: Q% d2 ^- b$ d+ x4 G5 ^
ADI值:不作限制。1 R& w' s% k. \! d7 f9 H
功能:着色剂+ W' A y Z k9 B' t& r2 i
8 @( F( p6 R) p# C0 J( ] X$ U
TITANIUM DIOXIDE
: s: @1 Q1 T2 M. {( U+ JPrepared at the 67th JECFA (2006) and published in FAO JECFA+ K; R: M, R/ c2 {
Monographs 3 (2006), superseding specifications prepared at the 63rd
! s$ ~ E* n0 a# d# S; lJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
" e* V* U" ?' F: J. j! j1 g, U, Y% p' MCombined Compendium of Food Additive Specifications, FAO JECFA
+ k% ~: P5 S& Y2 @Monographs 1 (2005). An ADI “not limited” was established at the 13th
7 n# q1 x' r, I/ U) nJECFA (1969).
& o& f& [( P" j, u; J; uSYNONYMS
; \: V% Y6 d& x, [) H) S! _Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
+ k4 [) O1 n( u/ m' T: JDEFINITION }* h+ _& \! ?$ @; J+ N+ d# F
Titanium dioxide is produced by either the sulfate or the chloride, T6 U: L' u& F5 H; W3 D" G
process. Processing conditions determine the form (anatase or rutile7 {- S- B1 d0 e' N1 ]2 U5 h+ F. Q
structure) of the final product.
6 k( E9 e( J& P' rIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
7 X' T# r& N- q- J- {5 G9 Mor ilmenite and titanium slag. After a series of purification steps, the
: H8 L0 x( K/ l ?( @& l/ u5 k) `isolated titanium dioxide is finally washed with water, calcined, and9 P) [5 h* _$ k- t' P
micronized.
8 B* g' } o1 Z7 N6 g7 R4 {8 D) \: QIn the chloride process, chlorine gas is reacted with a titaniumcontaining$ Q" e: n& R2 e! Z- M# @8 t3 p
mineral under reducing conditions to form anhydrous5 @1 L. O& Q u6 P8 f! d: Z
titanium tetrachloride, which is subsequently purified and converted to) h7 h/ y. l& g8 G& f3 _ s
titanium dioxide either by direct thermal oxidation or by reaction with
, J5 X. x2 X$ i% |5 Qsteam in the vapour phase. Alternatively, concentrated hydrochloric+ Y2 I( h' P1 Q
acid can be reacted with the titanium-containing mineral to form a9 R) T3 F# N9 p$ K+ q! I! ~
solution of titanium tetrachloride, which is then further purified and K% E8 i. V3 j# P" W: g
converted to titanium dioxide by hydrolysis. The titanium dioxide is
8 w, Q) e' q) Z0 F- T. Gfiltered, washed, and calcined.8 g$ H" o+ _+ w, |: s( L
Commercial titanium dioxide may be coated with small amounts of
( o/ s$ w* E3 ealumina and/or silica to improve the technological properties of the
6 c* D2 {; w, c3 r' q0 k! eproduct.0 U8 N0 y9 y( J! R, T! q
C.A.S. number 13463-67-7
" Y5 s9 r) U; w" ~/ T) Z0 LChemical formula TiO2
0 m* F/ b6 v8 h4 ?Formula weight
( p# a4 d) i7 _4 `& G! J0 K79.881 m6 d* ]1 @# o* C; H3 u# S/ }" B
Assay
. h+ F/ C1 i: ?9 x% K7 J( fNot less than 99.0% on the dried basis (on an aluminium oxide and6 H z% I+ c% a
silicon dioxide-free basis)4 N: o4 ]+ A( k: {
DESCRIPTION
+ u2 E4 `$ }- P4 h+ LWhite to slightly coloured powder
& z& E7 D a' O: I, XFUNCTIONAL USES
" c4 a1 i( L; r4 R/ ^# dColour, [% _' [/ f: x9 {
CHARACTERISTICS+ K9 A- w+ Y3 b: a1 j$ S
IDENTIFICATION
6 @* W. ]5 Y# J+ iSolubility (Vol. 4)
# U; J4 _) p* N7 LInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
( I6 b6 S4 |6 H" V5 D4 Z, g# xsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated0 ?. R% [ g; e; J
sulfuric acid.; C* {; Q6 O2 g
Colour reaction
8 |0 U4 y, |9 h3 ~+ B/ _) d# _( vAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
* h5 @5 K% T# M7 nsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
' J$ [9 l- Y* S# }. F- qwater and filter. To 5 ml of this clear filtrate, add a few drops of4 h# s& Y9 w/ @ p2 p0 |
hydrogen peroxide; an orange-red colour appears immediately.8 @; g, L: J3 k# c, Q
PURITY# {4 b/ U& L1 c p/ \$ L( }
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
! i% S( W! X/ J" }' jLoss on ignition (Vol. 4)$ k" D' z0 n) H% I; C
Not more than 1.0% (800o) on the dried basis
, Y! y- F8 W. C+ g9 M& x) WAluminium oxide and/or# o" g3 H+ T9 L7 u* d A
silicon dioxide% @$ z1 u7 _8 y
Not more than 2%, either singly or combined
* _( N3 p; l6 N: Z5 {8 ESee descriptions under TESTS5 D5 ?/ @; Z" X# A
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing' ~/ C' L7 e" w( t, G9 ]' r" G' U
alumina or silica.
3 \% U/ C* P4 d( } pSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and! g( I1 H+ Q- W7 e( S& M
place on a steam bath for 30 min with occasional stirring. Filter3 E5 t8 X4 f) K
through a Gooch crucible fitted with a glass fibre filter paper. Wash
- l, w* G1 d, s. j$ ~1 Owith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the0 r1 m9 J* M9 `2 h
combined filtrate and washings to dryness, and ignite at a dull red2 V3 o0 I7 N: _% h. l1 I
heat to constant weight.3 d' ~- m7 g& [" E' Z
Water-soluble matter( l Y, ]/ q P8 d
(Vol. 4)7 t2 g2 z n9 ~" D
Not more than 0.5%
% Z' ~6 Y/ W' cProceed as directed under acid-soluble substances (above), using
' Y# t2 z. Y" x5 dwater in place of 0.5 N hydrochloric acid.
6 J. }# _3 A+ f7 C8 Y8 \$ Q! TImpurities soluble in 0.5 N
5 {3 A S' Y3 W1 a$ N: vhydrochloric acid/ z" v* {3 b9 a7 t$ E- X5 I; ^$ h" ?
Antimony Not more than 2 mg/kg Z& ~. N' @1 S# q; ^! `
See description under TESTS" G+ n7 u( W2 K! O+ w; q3 a$ K& b
Arsenic Not more than 1 mg/kg
}9 O& v/ L( y- n! m8 |See description under TESTS
/ o# A. h$ s* n4 t+ SCadmium Not more than 1 mg/kg0 I* V$ g) T) |" H( W" O4 y" |0 h& W+ P
See description under TESTS
- h" e8 J* I& Y# Z1 H$ _& wLead8 l6 C, @- N& j+ V6 w8 B0 H' T. c
Not more than 10 mg/kg
. e/ ^+ k) {7 x! e SSee description under TESTS
' z9 }; l4 M' ^9 C) r9 OMercury (Vol. 4) Not more than 1 mg/kg
% o. W7 T- |7 Q$ P" b9 FDetermine using the cold vapour atomic absorption technique. Select a4 h/ d% k, Z& i0 ?1 Y7 i4 v% v
sample size appropriate to the specified level6 ~) @ X' t, @8 t: w) @
TESTS% c& E. T D T! w% p
PURITY TESTS7 z, m' M, _" Y: c# _9 B# V
Impurities soluble in 0.5 N
m- X- p1 j/ e4 F Ehydrochloric acid2 M4 s5 Y6 c! r/ M* ?; K
Antimony, arsenic,9 ]: r! y: Z* ?
cadmium and lead4 Z/ M# {* H7 k+ c. E
(Vol.4)
" e* ]4 C' [$ n5 M9 Q- BTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N# F6 f& d' |1 s9 K
hydrochloric acid, cover with a watch glass, and heat to boiling on a
+ T6 n. n: w- _3 ? B# whot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml4 G) g5 n( I! w3 J, P3 u. V
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
2 G8 X1 M8 L+ dmaterial settles. Decant the supernatant extract through a Whatman
5 U! ?& g+ C+ T% yNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml/ ], e2 H3 S( s5 g: `
volumetric flask and retaining as much as possible of the undissolved0 n1 \0 \% A* U" e7 M0 G6 @
material in the centrifuge bottle. Add 10 ml of hot water to the original8 |2 M( H5 `/ [& o
beaker, washing off the watch glass with the water, and pour the. @ r+ _2 }6 O7 Y h
contents into the centrifuge bottle. Form a slurry, using a glass stirring
o9 |, j& R3 mrod, and centrifuge. Decant through the same filter paper, and collect
2 z# w, | E0 W/ e$ fthe washings in the volumetric flask containing the initial extract.# x; P) ?3 B, o& i( J
Repeat the entire washing process two more times. Finally, wash the* _+ d# d* \4 Z2 H4 n' g
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask8 ^9 h0 }3 w( k
to room temperature, dilute to volume with water, and mix.
2 D% E0 b) S3 {& f5 `Determine antimony, cadmium, and lead using an AAS/ICP-AES) G1 ?$ r$ W0 k% @& ^
technique appropriate to the specified level. Determine arsenic using the: n7 ]' _7 r, Q. x k7 v
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using$ A! t- y5 Y9 q; Y2 b8 W$ S) a
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than( j3 T$ W1 c* Q, O( l: @
1 g. The selection of sample size and method of sample preparation
/ Q, l8 v7 _5 m1 J) xmay be based on the principles of the methods described in Volume 4.. t5 a0 x$ f5 `2 H" T* J
Aluminium oxide Reagents and sample solutions
7 l4 p4 N6 P i0 I. N0.01 N Zinc Sulfate
7 I- M4 P2 d9 d& G0 a2 @% BDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
1 [, R2 @% t' ~; ^- X4 Ymake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
+ ^. y; D9 p8 U9 }of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
2 N- l: i4 J) Zconcentrated hydrochloric acid, heating gently to effect solution, then
4 C3 T% L% U4 W# I/ g+ ]transfer the solution into a 1000-ml volumetric flask, dilute to volume" I% p0 Q/ M4 t4 x9 h4 S' c
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500. }' e5 E0 \2 q/ V9 \$ h# E& `
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
7 B1 c) E& o; _$ X2 \$ Pconcentrated hydrochloric acid, add 1 drop of methyl orange TS and6 K- Y9 u. k! H* ^; D8 r4 N* W' s
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
" l% |# w( `$ j0 Y! K3 [dropwise, ammonia solution (1 in 5) until the colour is just completely% }/ h+ f+ Z) [ ?; ?& G
changed from red to orange-yellow. Then, add:
' I- `) |, v6 n+ [1 C* u# O(a): 10 ml of ammonium acetate buffer solution (77 g of. m$ M& `4 }# t! c
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
$ M( c% @# y5 S& l4 A0 F9 D- |1000 ml with water) and
, q2 |! l& V, B7 w' n(b): 10 ml of diammonium hydrogen phosphate solution (150 g! F: f0 F, A- R) S0 T% N$ F$ V9 R
of diammonium hydrogen phosphate in 700 ml of water,
3 L# S% [0 E" Y+ Vadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
. ?; a+ Y( e9 }) G& t3 Fthen dilute to 1000 ml with water).
, n0 O4 H5 t4 s+ ^3 vBoil the solution for 5 min, cool it quickly to room temperature in a- e5 R) ]( f6 b7 s
stream of running water, add 3 drops of xylenol orange TS, and mix.
/ R( H! c8 F4 s: NUsing the zinc sulfate solution as titrant, titrate the solution to the first
6 i) w$ \: S7 D- F3 fyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
- J. o( G% F! e* M* U) u# F5 F6 ?: `This titration should be performed quickly near the end-point by
8 D! W A! S) s* L. F. Dadding rapidly 0.2 ml increments of the titrant until the first colour
4 u" w/ g/ \1 j% [$ X, E, Zchange occurs; although the colour will fade in 5-10 sec, it is the true
. _" O5 [4 R/ L3 }9 Rend-point. Failure to observe the first colour change will result in an' H" k1 A/ V. Q3 a8 P0 `
incorrect titration. The fading end-point does not occur at the second
: P* w6 m% F: Q8 \( Bend-point.)
7 D' o& s1 H* }* \& Z' V0 R) gAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
8 C! K! ]9 G% C$ Y6 ^, Nstream of running water. Titrate this solution, using the zinc sulfate: O: l' w1 [- W/ l b' H
solution as titrant, to the same fugitive yellow-brown or pink end-point% B9 Q' @7 S* w3 i- c; }7 N
as described above.
1 k2 w% e% n* B2 D! {0 bCalculate the titre T of zinc sulfate solution by the formula: k: s+ F$ {. l( V1 J. x$ S
T = 18.896 W / V. _' k4 ] Z' ]7 o% i: q
where
1 Z/ I9 ?8 x6 k8 M' h9 G. lT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
' Y4 r6 L a6 @ Y0 N2 g2 vW is the mass (g) of aluminium wire6 O f9 ?: K8 E( p- u
V is the ml of the zinc sulfate solution consumed in the
) ? \* A% l) ^6 Z+ z) Xsecond titration
6 ^3 q$ v: p- y0 R18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and, i$ y& {" k7 j' O& O6 F
R is the ratio of the formula weight of aluminium oxide to
, B# M6 ~: e* Y% V+ W: ]that of elemental aluminium.
9 R5 f; M+ f/ E# W9 p' o. P6 ISample Solution A
6 A) s& N& V! d7 W# Z: N% V* `Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
/ l9 N& T! e- l) Q7 Gglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).0 k M( S+ z `3 `
(Note: Do not use more sodium bisulfate than specified, as an excess
# L" a& b1 N% J" i$ T* rconcentration of salt will interfere with the EDTA titration later on in the; @. V: ?2 [( w. v/ u9 @) ^. B
procedure.) Begin heating the flask at low heat on a hot plate, and
. S2 m4 {6 i/ Q! h% Pthen gradually raise the temperature until full heat is reached.
0 G0 y3 K6 g# Z* u(Caution: perform this procedure in a well ventilated area. ) When, Y: F1 u6 X" E c
spattering has stopped and light fumes of SO3 appear, heat in the full
0 f: h& C$ V: }$ J/ U4 Q8 hflame of a Meeker burner, with the flask tilted so that the fusion of the/ h( g8 U! T, h
sample and sodium bisulfate is concentrated at one end of the flask.9 B7 e$ U' O' Y& ~! K
Swirl constantly until the melt is clear (except for silica content), but
& n \- l5 ?# ?; W( b$ nguard against prolonged heating to avoid precipitation of titanium
6 t; @. g* l; i A# i; Ldioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
1 d; [; y m& x: V2 _the mass has dissolved and a clear solution results. Cool, and dilute to5 h% [, m) {) {- `" _0 v5 ]9 v
120 ml with water. Introduce a magnetic stir bar into the flask.$ n; H, _" o' P6 R6 V H6 \
Sample Solution B
! [5 r" u6 X0 D# A6 @4 uPrepare 200 ml of an approximately 6.25 M solution of sodium% u/ ]% e* G* ]
hydroxide. Add 65 ml of this solution to Sample Solution A, while
6 o. L P. y' B5 D3 ^9 @0 zstirring with the magnetic stirrer; pour the remaining 135 ml of the
* T$ n) \1 |5 zalkali solution into a 500-ml volumetric flask.
( O# R3 x& _/ h7 z; R W, \$ s/ v( a, tSlowly, with constant stirring, add the sample mixture to the alkali
* `' L$ G# F$ U4 c# A8 c3 ~ K1 xsolution in the 500-ml volumetric flask; dilute to volume with water,
2 ~# j. a' l& E6 y5 s6 d2 Eand mix. (Note: If the procedure is delayed at this point for more than/ ?, r3 u. k* [2 P; L
2 hours, store the contents of the volumetric flask in a polyethylene
, \/ X' M4 s8 S* `3 p- cbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
4 l! O* M/ H$ w$ n& N, Xthen filter the supernatant liquid through a very fine filter paper. Label
9 \% U% H( }. ^$ T" {% Sthe filtrate Sample Solution B.# U' r8 ^1 Q4 }3 p: m5 I- B
Sample Solution C
h8 i9 O6 @9 S% H: STransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer3 I3 a1 ^% Y& Z c
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid5 B* d" _3 l( b
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
N' [& C4 U6 [; k' j& zM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
7 M, X" U6 Q) Y2 g, Pknown, calculate the optimum volume of EDTA solution to be added% j$ Q% a. C3 x: V6 J4 ^
by the formula: (4 x % Al2O3) + 5.]
( V0 ^* @& C+ N* D0 i: wAdd, dropwise, ammonia solution (1 in 5) until the colour is just
* c. } c6 |* ?8 i- Icompletely changed from red to orange-yellow. Then add10 ml each3 j! k3 [- R) G. P* ?& p
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to# }; c; b! n* |8 A
room temperature in a stream of running water, add 3 drops of xylenol
1 D4 y1 J" Q; t8 a0 d5 |' Eorange TS, and mix. If the solution is purple, yellow-brown, or pink,3 S( s% X% P5 M5 f& E5 Q
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
7 E; k% Y" r M4 ?pH, a pink colour indicates that not enough of the EDTA solution has
9 Y$ L: K$ ?6 k0 jbeen added, in which case, discard the solution and repeat this
0 s" T4 e/ D2 aprocedure with another 100 ml of Sample Solution B, using 50 ml,
) H7 P6 ]8 m$ ]7 i5 k. H* Drather than 25 ml, of 0.02 M disodium EDTA.
! p# r/ [0 o; e5 W- b; LProcedure
; w4 m- ~4 o- y( RUsing the standardized zinc sulfate solution as titrant, titrate Sample& L$ N5 S- [( _3 y( v# s* r
Solution C to the first yellow-brown or pink end-point that persists for: {6 E1 Y! G5 b
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first' X3 T5 v+ }3 f; x4 y7 g
titration should require more than 8 ml of titrant, but for more accurate& V' p2 I( i# @4 \/ X! u
work a titration of 10-15 ml is desirable.' G* o2 M8 H0 _5 {7 h+ ~
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5! h# D5 Q( [% S1 A/ n8 i- a
min, and cool in a stream of running water. Titrate this solution, using
, \1 J3 b7 x0 c# N$ d7 ~the standardized zinc sulfate solution as titrant, to the same fugitive+ g! D4 I+ d5 a$ u |
yellow-brown or pink end-point as described above.
! J W1 c; V* tCalculation:5 P" K' u: `4 A7 x$ \3 @
Calculate the percentage of aluminium oxide (Al2O3) in the sample
$ Z0 X: L+ G |! H H' [taken by the formula:
8 T: Q3 K5 O( j' S5 f4 r: q% Al2O3 = 100 × (0.005VT)/S
+ |9 n# c0 D. r( F$ Iwhere' B" `1 ?7 ^; I1 W- a: ~
V is the number of ml of 0.01 N zinc sulfate consumed in) W. j/ \9 _, O( J, W. @; {% r$ Y
the second titration,
& \7 u; Q O% s8 X# T1 ]. eT is the titre of the zinc sulfate solution,0 g% V* {2 g. W4 n4 r* y
S is the mass (g) of the sample taken, and5 R; {9 j8 _- F. q- e* Y
0.005 = 500 ml / (1000mg/g × 100 ml).3 [7 L, c! `. ~/ O, s2 n5 n
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
; d; [/ o; V o! m* t0 jglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).% m0 u& g9 p1 v. A
Heat gently over a Meeker burner, while swirling the flask, until( u; ?5 ^" K- e7 k2 m& `7 S4 w; u
decomposition and fusion are complete and the melt is clear, except
& [. u, w2 F- b3 k- bfor the silica content, and then cool. (Caution: Do not overheat the
6 ]/ ?: r! R; x/ c% |contents of the flask at the beginning, and heat cautiously during
. I6 C8 R) Y' k6 V# A3 K4 vfusion to avoid spattering.)
- S- D" `7 m! I$ tTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat. E+ K& U+ K8 k- X& s8 C
carefully and slowly until the melt is dissolved. Cool, and carefully add% D. }& {9 l% J$ S
150 ml of water by pouring very small portions down the sides of the5 {* _ V k4 l; z' A
flask, with frequent swirling to avoid over-heating and spattering. Allow
% s5 k( w- d7 x! a5 ~the contents of the flask to cool, and filter through fine ashless filter
/ I! r+ p% ?( W& r: t0 N1 e0 npaper, using a 60 degree gravity funnel. Rinse out all the silica from, [* l* D8 D/ L$ {4 w' ?
the flask onto the filter paper with sulfuric acid solution (1 in 10)." `* u* S* r/ V7 g8 C: L4 _ f
Transfer the filter paper and its contents into a platinum crucible, dry in
8 r" }; c# }' e+ Dan oven at 1200, and heat the partly covered crucible over a Bunsen# g: N5 ~1 R% y8 w
burner. To prevent flaming of the filter paper, first heat the cover from$ c% X+ ]( d7 X) f6 ^
above, and then the crucible from below.
2 {! u8 j" q. J/ x6 I( aWhen the filter paper is consumed, transfer the crucible to a muffle
" l" H/ Z' t% m* }# u5 wfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and, ~" U( Y) C; D1 P5 k4 F
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated5 ^: I' N$ d& D) Q9 M
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
+ S; [: z) [/ jon a low-heat hot plate (to remove the HF) and then over a Bunsen
3 S. A; o& a3 {* xburner (to remove the H2SO4). Take precautions to avoid spattering,
, D# P0 \8 F4 Q. uespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
1 F* C) ?: P" E* D/ Fdesiccator, and weigh again. Record the difference between the two3 ?( K) |5 {; w/ [
weights as the content of SiO2 in the sample.
8 s" n+ t" e8 S3 q1 Q7 dMETHOD OF ASSAY9 D: d1 s8 L' r6 o
Accurately weigh about 150 mg of the sample, previously dried at 105o
3 V! e* f! _+ [4 D% kfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
W( Q7 h) j# U+ [8 xand shake until a homogeneous, milky suspension is obtained. Add 30
, s5 U: o6 v; X" z* a* |, G7 |ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
' \0 S2 c8 W) R& C6 I! Bheat gently, then heat strongly until a clear solution is obtained. Cool,
; `* N( `3 u0 m! a+ Y; Z5 Jthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric0 ?+ ]8 n0 s$ M
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
! j) u9 k& T! brubber stopper fitted with a U-shaped glass tube while immersing the* T) g! g" ^+ |( Y$ h
other end of the U-tube into a saturated solution of sodium4 M" a+ F. O6 ]
bicarbonate contained in a 500-ml wide-mouth bottle, and generate+ x) H5 P0 @" z) _6 r$ y
hydrogen. Allow to stand for a few minutes after the aluminium metal
4 y3 G% ]0 t8 i/ M Y6 W; W5 V- Hhas dissolved completely to produce a transparent purple solution.5 h6 x' t9 p ?6 T) S$ K& E1 K
Cool to below 50o in running water, and remove the rubber stopper
* Y) d {- ?$ H5 p: p8 e4 scarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate e% m1 ?$ J& i; S4 `6 l' M$ `
solution as an indicator, and immediately titrate with 0.2 N ferric0 J4 x' ^* L! O/ V
ammonium sulfate until a faint brown colour that persists for 301 M$ L1 g' G2 a8 Z
seconds is obtained. Perform a blank determination and make any
( @" V1 C9 F8 |% @3 S( p4 Qnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
3 o4 D! M3 L" q. r+ Dequivalent to 7.990 mg of TiO2.& d$ p3 s3 P% k1 J7 P0 f# k( z
|
|