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二氧化钛(钛白粉)
二氧化钛(钛白粉)! w! t2 W" v. g3 t. l* f8 v
# d8 ~: P* A3 r* U. I# O2 iJECFA关于二氧化钛(钛白粉)的结论
9 Q2 u* z- @3 Z( d) S
' _5 p0 T; u2 P& B1 k摘要: 2006年JECFA关于二氧化钛的结论
- |, G9 ^- x% G- b; {& Q" c0 e1 GADI值:不作限制。
; r4 ?1 a+ i8 J: [# |2 [: r6 \5 `8 ~$ P功能:着色剂5 D2 V3 |) a/ e7 ]
+ e2 i+ _/ p8 A2 U7 ?. W2 { p1 ~* `TITANIUM DIOXIDE
+ x/ e' V4 G8 ^. m9 QPrepared at the 67th JECFA (2006) and published in FAO JECFA/ j) w# N5 e1 q7 u: e
Monographs 3 (2006), superseding specifications prepared at the 63rd
2 }, z- e5 U/ ~: AJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
% v% d( X6 f1 k5 YCombined Compendium of Food Additive Specifications, FAO JECFA
+ ` t5 k( W$ y" m( q( b6 O1 ^Monographs 1 (2005). An ADI “not limited” was established at the 13th% T0 A* @7 G" M- [
JECFA (1969).$ @3 V3 F& ]9 h/ b
SYNONYMS8 U. l% [. P: |7 J: Y
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171' a- o4 ^9 `8 A4 N0 C
DEFINITION) k' x* a7 j5 ~, p' M! x- k
Titanium dioxide is produced by either the sulfate or the chloride
, n0 k4 r$ M; q% `8 b! t' i$ s' @process. Processing conditions determine the form (anatase or rutile
; ~* j/ C/ J( G( e. h" lstructure) of the final product.
1 f: {3 b; ~6 x/ JIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)! N. D0 G4 s9 x( T; c* Z
or ilmenite and titanium slag. After a series of purification steps, the
: Q3 c: h/ }/ G% G, ^9 Pisolated titanium dioxide is finally washed with water, calcined, and
& T# R9 L; n1 V0 {+ W* umicronized.4 m5 X( z8 k7 S% a! y4 k Y
In the chloride process, chlorine gas is reacted with a titaniumcontaining
4 F- M" ?) ?. t- k( N9 Ymineral under reducing conditions to form anhydrous) [, Y3 ?7 P; C) B% X; S4 p
titanium tetrachloride, which is subsequently purified and converted to
$ Y4 Z* w1 p* s* q) Htitanium dioxide either by direct thermal oxidation or by reaction with
% ~' E4 D2 U' w4 x' P1 O$ v3 _$ X/ vsteam in the vapour phase. Alternatively, concentrated hydrochloric" C7 [! l/ }8 s6 t: \6 W1 Y
acid can be reacted with the titanium-containing mineral to form a2 `( g8 D% u8 l6 C0 p
solution of titanium tetrachloride, which is then further purified and4 X+ |+ r0 j0 t6 k f# ]- j
converted to titanium dioxide by hydrolysis. The titanium dioxide is
$ ?, W" h% \. p3 C/ U+ p3 T% Ifiltered, washed, and calcined. }7 b: x4 o' ?; r: p) x
Commercial titanium dioxide may be coated with small amounts of- b: p* ]8 N* T9 j4 U. a
alumina and/or silica to improve the technological properties of the/ ]& g j$ G8 b! o
product.
0 o8 }: M2 R& JC.A.S. number 13463-67-76 B5 T# ^6 u9 S6 @& k7 N1 N1 d1 d
Chemical formula TiO2
# F. j) X3 j) z' o$ j! e CFormula weight
9 J" Q1 Z( J# \3 D0 R/ ^ [+ j79.88% ?, f: x& y. g7 r1 K+ C
Assay3 A1 B% G: N# P2 N3 d
Not less than 99.0% on the dried basis (on an aluminium oxide and
, q6 c/ T1 c3 R6 Nsilicon dioxide-free basis)9 ^! _5 L' T- K$ w& ~
DESCRIPTION
" z: m6 E% U8 F2 i/ pWhite to slightly coloured powder# N( D0 b7 h- }' a, C5 D
FUNCTIONAL USES
% F, L" k' y# tColour
2 ^+ |! d1 { m9 b: Y- A' s1 dCHARACTERISTICS
" \% C5 _# T* J8 v3 i3 o" o+ R" C- }6 _IDENTIFICATION8 @/ ~ b- s0 h1 E! ]& _; u
Solubility (Vol. 4)
2 L, S7 S7 @8 B9 \Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
/ e% X8 i3 \/ k# F2 M+ r1 `solvents. Dissolves slowly in hydrofluoric acid and hot concentrated& [: F* c; k- m/ }0 Q7 ^" l
sulfuric acid.: f4 w% w) f8 z' Q. x8 G
Colour reaction
/ u# U; ~; u C; rAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of: ^& c9 x4 E! z
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with0 j, {3 Q0 G" r6 _. H
water and filter. To 5 ml of this clear filtrate, add a few drops of- l8 b& D* l. l9 i7 ]' |0 U
hydrogen peroxide; an orange-red colour appears immediately.
# L8 N7 S1 X- V/ ~" c( h" tPURITY g8 G/ {3 u* ~0 B8 a4 G
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h): Q$ m" ~; o7 S" ~ c+ \) r
Loss on ignition (Vol. 4)3 v, Z( i' `' S- ^
Not more than 1.0% (800o) on the dried basis+ h' y! j( K/ M$ t8 m) Y) v
Aluminium oxide and/or
1 x2 C7 Z, e3 D [, M& \( d4 z5 Esilicon dioxide2 R! N( \% h% Z6 C' F: `
Not more than 2%, either singly or combined
' X% c- o, M& S5 Y) x4 ?' e% u/ SSee descriptions under TESTS, E& }( ?# W, S3 z7 v. B5 \! h
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing/ ]; s4 e+ Y: J! W; R! v
alumina or silica.
) T/ p; y: l' [0 |Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and3 W7 h. Q- ~- q% b' Q
place on a steam bath for 30 min with occasional stirring. Filter, `& q- X% h! _- d8 M+ M" A( Z* B
through a Gooch crucible fitted with a glass fibre filter paper. Wash" j9 k/ L0 N3 D! _, }8 U/ I) ~
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the+ C& ^1 l( D, n" F1 [" I
combined filtrate and washings to dryness, and ignite at a dull red
# n) R# Z9 l! z" r. xheat to constant weight.
7 ^2 V/ A0 r* z7 e. m m4 ~. bWater-soluble matter
9 X$ }3 p; d( ]0 t& _(Vol. 4)# L& N5 j; Z! t
Not more than 0.5%
! q6 d+ n; }; A, v. @6 H- ]Proceed as directed under acid-soluble substances (above), using
2 ^8 V& V: s3 L# I9 d# Ewater in place of 0.5 N hydrochloric acid.* I+ B4 v# ^) i' c& G6 ]
Impurities soluble in 0.5 N
; s4 W3 L0 ?7 B- i: Yhydrochloric acid7 S) N" ~/ x: F( K0 u
Antimony Not more than 2 mg/kg( L" h* `$ r8 q. E. t! G ?
See description under TESTS
5 c8 N0 L0 S A! g+ n {' sArsenic Not more than 1 mg/kg
2 j, v2 |& m6 L2 _See description under TESTS* D* H$ g2 z" }
Cadmium Not more than 1 mg/kg# B- j! o8 x/ n6 {( q8 S
See description under TESTS7 z' [4 P, ^6 L1 R
Lead# s2 [& k$ t) `, q6 m
Not more than 10 mg/kg4 [9 x$ e+ @! s- }9 |
See description under TESTS* ?& L1 b9 Q% d ~4 t) i" V3 n! Z
Mercury (Vol. 4) Not more than 1 mg/kg9 [4 E8 A: Q* L* k
Determine using the cold vapour atomic absorption technique. Select a& P6 L6 y+ y- v2 k
sample size appropriate to the specified level
9 v5 T- ?$ x/ d7 ZTESTS2 `5 F" Q6 ]- t, t) v/ r
PURITY TESTS% K* ^: ^% J1 q g' W
Impurities soluble in 0.5 N* g# B2 i9 F p( T: c' C! y5 Y# ~& J
hydrochloric acid
7 w; o: V+ A9 N6 H# X5 YAntimony, arsenic,3 i9 w' y. N0 g+ Z$ W
cadmium and lead6 W; s) \0 J/ T2 m# m0 o
(Vol.4)* ?# y( R f0 U F% V0 F
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N3 w. w) a7 `1 c2 t
hydrochloric acid, cover with a watch glass, and heat to boiling on a
5 U; E- ]- O8 E5 _hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml# k- W% S6 J5 p( C f$ p# e
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
$ ?1 a) _% V5 C9 jmaterial settles. Decant the supernatant extract through a Whatman
7 K8 U& g' Y+ F0 v6 eNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml# w5 }% ~8 V: c
volumetric flask and retaining as much as possible of the undissolved9 ]1 p$ ]% W+ a+ z E
material in the centrifuge bottle. Add 10 ml of hot water to the original
# C% k4 C+ D4 V2 y& s9 Z% m- n5 u/ pbeaker, washing off the watch glass with the water, and pour the
j1 G* l6 M* \contents into the centrifuge bottle. Form a slurry, using a glass stirring' M9 c/ ~8 T! q2 R. n. \
rod, and centrifuge. Decant through the same filter paper, and collect `9 N+ w0 r) d% P! t$ @2 M
the washings in the volumetric flask containing the initial extract.! e, q& _+ D9 {4 l) L3 H" |
Repeat the entire washing process two more times. Finally, wash the# I9 \# A! q. U3 `$ B6 i B7 w2 D0 i
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask! S6 ^4 \% \+ T0 m
to room temperature, dilute to volume with water, and mix.7 x) h. {/ v* n z& c
Determine antimony, cadmium, and lead using an AAS/ICP-AES/ `8 @$ z. Q) i+ p- T$ F
technique appropriate to the specified level. Determine arsenic using the
5 {0 p% `) }) ]7 _, N8 YICP-AES/AAS-hydride technique. Alternatively, determine arsenic using* `2 N, L8 b& a) B" P
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than$ V: t: {" ~2 W9 n
1 g. The selection of sample size and method of sample preparation5 T& t6 g# H) b5 X
may be based on the principles of the methods described in Volume 4.* f' ^+ W6 W6 { g$ k7 F( J) W6 w
Aluminium oxide Reagents and sample solutions9 [ Y! T% q+ q) v5 D
0.01 N Zinc Sulfate9 h% R9 W3 K8 x+ {
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
3 ^1 t/ _0 C4 lmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg$ E: K( V7 u( W: U. z
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of8 W4 i3 x3 x0 v* P
concentrated hydrochloric acid, heating gently to effect solution, then5 Q7 z+ ~, s$ |5 V9 p$ |) p: P
transfer the solution into a 1000-ml volumetric flask, dilute to volume; {2 ^" i) C" d% J2 m; {3 w* M
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5009 C5 l1 _6 y# {( u/ _+ Z
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
1 t* e+ E4 j Wconcentrated hydrochloric acid, add 1 drop of methyl orange TS and- m* ~; `) ]/ m" t1 ]4 F; }
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,& L" R5 ^( E: a* }
dropwise, ammonia solution (1 in 5) until the colour is just completely$ S# V* t* c1 E! h' F3 f9 O* J
changed from red to orange-yellow. Then, add:- o" L& O1 t J# [: w( j& X% [
(a): 10 ml of ammonium acetate buffer solution (77 g of5 D, E; V) I3 k* |) ]
ammonium acetate plus 10 ml of glacial acetic acid, dilute to$ i: L) c! r1 T; @2 b
1000 ml with water) and# K# N( a) q B6 m) L
(b): 10 ml of diammonium hydrogen phosphate solution (150 g: ^1 L9 q3 h& j) {! T
of diammonium hydrogen phosphate in 700 ml of water,
; t1 I5 k, P1 r J* x- X6 Kadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
+ E! S& O* i. `2 lthen dilute to 1000 ml with water). _6 i5 \* K4 `7 A) ]
Boil the solution for 5 min, cool it quickly to room temperature in a f& N1 m1 Z. h( @! ], {( m
stream of running water, add 3 drops of xylenol orange TS, and mix.$ O8 g& H: l7 ?, t) J3 N: B
Using the zinc sulfate solution as titrant, titrate the solution to the first3 E7 J- k3 j% h4 l" `
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
# R# S' x8 E, g9 y9 i" iThis titration should be performed quickly near the end-point by
$ f$ o9 f3 H: I( s- b, h5 ~4 S- t( Sadding rapidly 0.2 ml increments of the titrant until the first colour3 _/ q$ W/ Y& G( w
change occurs; although the colour will fade in 5-10 sec, it is the true
2 @8 X0 a' l" h) n" v$ v5 G' Nend-point. Failure to observe the first colour change will result in an
# g) Q, W4 T9 s5 u9 ?incorrect titration. The fading end-point does not occur at the second
, ` Y( u7 r) a& k: Gend-point.)
" J6 J9 ]9 {# ]: b" nAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a# C- N1 k6 }% y1 m$ U
stream of running water. Titrate this solution, using the zinc sulfate3 J$ R% C/ C; \- t
solution as titrant, to the same fugitive yellow-brown or pink end-point
% W1 Z, O0 Y+ u' v+ [as described above.# v5 c7 ]" Q, N6 `- S
Calculate the titre T of zinc sulfate solution by the formula:. w& ?+ K" Y6 c4 Z3 J' I
T = 18.896 W / V! E$ i. M4 V r# M! [6 Y. w: F
where0 s1 s. H2 Z7 r8 ^) R
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution0 I7 G7 W( B7 M" N, C+ r. @
W is the mass (g) of aluminium wire: q! x: s: G7 H2 n6 T- x$ [
V is the ml of the zinc sulfate solution consumed in the& R( f- D+ Z+ p0 a, o
second titration
5 N( I$ A' | _8 R1 V" E6 O% \1 A18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and6 l) A0 ~, w% p' R+ Z- f
R is the ratio of the formula weight of aluminium oxide to5 W( p( K8 w% d3 c) h( x8 p
that of elemental aluminium.
& f) B' t; M1 S' ?* hSample Solution A& C: P/ W5 {% O- ~) U! w; x
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica* g/ [4 R+ c- K" I y- u) G
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
( t, }$ G$ m' |(Note: Do not use more sodium bisulfate than specified, as an excess" y- q) N# \1 b9 `& s" y
concentration of salt will interfere with the EDTA titration later on in the3 C! H9 r. y) B" g& @
procedure.) Begin heating the flask at low heat on a hot plate, and) T: a. w( J& E5 j5 I2 e }
then gradually raise the temperature until full heat is reached.! W, I& ?! z1 W Z
(Caution: perform this procedure in a well ventilated area. ) When( e( A# `! {- O
spattering has stopped and light fumes of SO3 appear, heat in the full
: y8 l7 n6 y! b2 T0 @% gflame of a Meeker burner, with the flask tilted so that the fusion of the& Y4 w, f% A0 j7 \2 ?7 ]. q
sample and sodium bisulfate is concentrated at one end of the flask.
& ^3 c) [: Y8 XSwirl constantly until the melt is clear (except for silica content), but3 z& ~1 D% T( ]( r2 [6 ]0 \, w
guard against prolonged heating to avoid precipitation of titanium* s) ^7 N3 Z; K" p' e I
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until9 j- L T v, R' L( b
the mass has dissolved and a clear solution results. Cool, and dilute to
4 b5 Z) q- [6 Z+ s120 ml with water. Introduce a magnetic stir bar into the flask.
0 n$ ?! ]! {* p" g0 USample Solution B$ N* _0 |. ]/ E, c
Prepare 200 ml of an approximately 6.25 M solution of sodium
: m, R% [) L8 X, O2 {5 nhydroxide. Add 65 ml of this solution to Sample Solution A, while
9 z7 o# u: O, G1 U* Z; l. Wstirring with the magnetic stirrer; pour the remaining 135 ml of the
! ?" Y8 x. R7 O, {alkali solution into a 500-ml volumetric flask.
$ Q' L/ {' _6 K8 QSlowly, with constant stirring, add the sample mixture to the alkali, O* f$ h' m: |( \, m# E$ ]4 {
solution in the 500-ml volumetric flask; dilute to volume with water,
% x8 L: {" |- v% V2 T7 ]and mix. (Note: If the procedure is delayed at this point for more than
7 ^/ O( u8 A7 p2 hours, store the contents of the volumetric flask in a polyethylene
# C5 w, o% ^ j1 k! U* bbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),. o+ E$ P0 E1 z$ j' V) H
then filter the supernatant liquid through a very fine filter paper. Label
8 o) e% m# i0 b5 [2 E& Q; T/ Hthe filtrate Sample Solution B.
! A" Z, r( l* T G& q4 h* p6 LSample Solution C
5 E' k* v; r/ |8 d! eTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
9 I% C1 ]0 K! E+ hflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid1 V! I1 r4 Q5 S7 g5 ~5 [7 K( H$ g
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02' a- ~+ _8 m6 T+ ~! m1 n
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is+ O+ @+ a( `: ~; L# V
known, calculate the optimum volume of EDTA solution to be added2 S% l7 G3 ^% P( B1 H g. C1 V# f
by the formula: (4 x % Al2O3) + 5.]' x( K$ E, m0 r C5 [, ]
Add, dropwise, ammonia solution (1 in 5) until the colour is just& V! ]2 x! L+ W( J n; K
completely changed from red to orange-yellow. Then add10 ml each
+ @" v/ e0 I" O0 x3 H$ \( C: ]of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
* R0 R5 G# r. X9 a3 U& O0 Rroom temperature in a stream of running water, add 3 drops of xylenol' O+ S; B; g6 d! \
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
- o) r" y l' w% m |* f8 S) W/ hbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
) Y3 j: O/ g0 v" j+ g7 }pH, a pink colour indicates that not enough of the EDTA solution has: y0 V* J/ r J! d- ]1 ^
been added, in which case, discard the solution and repeat this8 z3 f7 V8 w0 Z: C- \4 n7 K
procedure with another 100 ml of Sample Solution B, using 50 ml,5 A. q0 u* N4 b+ d: ?2 f, M
rather than 25 ml, of 0.02 M disodium EDTA.
% W; k& @. K) c! a" S' hProcedure
9 y# H6 M( W8 g( g% zUsing the standardized zinc sulfate solution as titrant, titrate Sample
1 N% h; w+ w! H6 G6 p2 gSolution C to the first yellow-brown or pink end-point that persists for
5 s6 B1 U: o4 \5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first' T: a2 A) I1 n7 U o8 B
titration should require more than 8 ml of titrant, but for more accurate1 ]8 O/ ~) c( Z
work a titration of 10-15 ml is desirable., V5 y5 y1 z5 u& ?- r" H) {: V
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5' {8 F5 f5 ~" k
min, and cool in a stream of running water. Titrate this solution, using
9 O+ J4 V _' z" ]. x4 Q& `$ Nthe standardized zinc sulfate solution as titrant, to the same fugitive# p* p' T! R9 o; j9 }$ L- R2 a
yellow-brown or pink end-point as described above.# p) |; C" E0 j* r0 _
Calculation:
! \ O6 D0 U& |Calculate the percentage of aluminium oxide (Al2O3) in the sample
- o2 u, |% @, c: @; P6 etaken by the formula:
: M% `% W& R9 w% D/ l& L" n8 J% Al2O3 = 100 × (0.005VT)/S( B! a! N0 j( b: w5 a
where
. ]* Z5 z! }9 a1 L4 t; k* j+ }V is the number of ml of 0.01 N zinc sulfate consumed in' p- l" U3 d# g0 S$ }- Q$ z
the second titration,& p8 _7 e" B+ I
T is the titre of the zinc sulfate solution," q3 D k1 s8 n' D' ~2 `
S is the mass (g) of the sample taken, and4 n) k! I( I# j1 y
0.005 = 500 ml / (1000mg/g × 100 ml).
: x( N2 L/ m0 ^* g, USilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
7 q4 N5 C% H" V! [* I3 `glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
/ [' b* E, u$ r+ Z2 A/ @4 [" ?Heat gently over a Meeker burner, while swirling the flask, until$ K4 K1 ^0 u9 X4 e
decomposition and fusion are complete and the melt is clear, except
; P" e( Q1 V& l8 W gfor the silica content, and then cool. (Caution: Do not overheat the6 F5 k2 v _ [9 _9 b3 G) b# B
contents of the flask at the beginning, and heat cautiously during* k# v# O) K# B4 T! K( l+ I
fusion to avoid spattering.)7 U7 I7 W% y8 v4 m3 E4 r
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat( q$ c+ `& Y5 k/ }8 ?( W" A& X' }0 y
carefully and slowly until the melt is dissolved. Cool, and carefully add
6 I8 p2 w0 J) }; W' c% U150 ml of water by pouring very small portions down the sides of the
/ r( z0 E$ ~9 j7 e& J! g5 xflask, with frequent swirling to avoid over-heating and spattering. Allow( e3 f* p2 G% x' ~7 \6 c' V+ s
the contents of the flask to cool, and filter through fine ashless filter$ H& K! u/ F) n1 r
paper, using a 60 degree gravity funnel. Rinse out all the silica from" F3 {2 B4 w' q: `4 q/ c; c l
the flask onto the filter paper with sulfuric acid solution (1 in 10).2 I7 X9 Y }0 c( p, Q& d: G
Transfer the filter paper and its contents into a platinum crucible, dry in' B) [9 ?: a) o- F/ D( ]8 Q/ {# G9 S
an oven at 1200, and heat the partly covered crucible over a Bunsen/ n0 H+ x. ^8 b* G7 |
burner. To prevent flaming of the filter paper, first heat the cover from |# g' j! E; g* q! D2 O
above, and then the crucible from below.
) Q, x6 n& s+ G/ RWhen the filter paper is consumed, transfer the crucible to a muffle
1 W& g/ y/ c+ _3 \! F' Gfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
! B7 g5 {% F o$ E* dweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated% G2 o8 h/ J# Y+ q" l- I3 N V
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first2 G2 q3 w3 U- |4 p1 \$ f
on a low-heat hot plate (to remove the HF) and then over a Bunsen
4 I! P! {- k& Q) @; Q: fburner (to remove the H2SO4). Take precautions to avoid spattering,$ d5 L: p9 `& d3 y" L2 ^/ Z
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
6 \" F: X" E n5 k; B3 ~0 Wdesiccator, and weigh again. Record the difference between the two
) |- R8 X7 o: N) @+ ]2 d+ [weights as the content of SiO2 in the sample.2 q5 R7 h; a0 v4 }* S0 u p$ `: H
METHOD OF ASSAY L3 F. g" K F9 ~5 |9 i( Q% V3 e3 o/ F
Accurately weigh about 150 mg of the sample, previously dried at 105o ?& V# h4 U H; k# |8 _
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
2 G2 b, A) \( F$ v% O% z( U. aand shake until a homogeneous, milky suspension is obtained. Add 30' {. L6 w$ a6 o( m* p' d
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially4 }& {4 r( c6 {8 }. o; u
heat gently, then heat strongly until a clear solution is obtained. Cool,
9 t" N P7 }1 H# O& S3 Dthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
0 [4 {2 G$ @1 v% w+ C/ ^1 D; vacid, and stir. Add 3 g of aluminium metal, and immediately insert a$ a; U* O/ C% `* j* H' [- D
rubber stopper fitted with a U-shaped glass tube while immersing the
# c5 T) D5 Z' P4 I% u+ hother end of the U-tube into a saturated solution of sodium
. i5 o0 F7 h8 ibicarbonate contained in a 500-ml wide-mouth bottle, and generate
' E0 t8 M: g3 c1 F8 F- Nhydrogen. Allow to stand for a few minutes after the aluminium metal. ^$ P; B% k, T- c, _6 y6 l
has dissolved completely to produce a transparent purple solution.
% {$ `& d& f9 y7 I' ]6 `Cool to below 50o in running water, and remove the rubber stopper
- v5 }/ E/ T, K4 @4 X* b Z6 |carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate. u2 O' D; v" L6 [
solution as an indicator, and immediately titrate with 0.2 N ferric& P( o3 L9 x N9 Y8 y
ammonium sulfate until a faint brown colour that persists for 30
2 y9 o* i2 K8 u9 Q4 A2 O( @1 ?seconds is obtained. Perform a blank determination and make any
- q& U6 t* s; ?6 S) b' }6 Anecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
) {! U7 n1 `2 K9 X* V4 p6 P Zequivalent to 7.990 mg of TiO2.
) U/ s4 w& l+ Q+ X. m( U! E |
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