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二氧化钛(钛白粉)
二氧化钛(钛白粉)
0 r+ y# A: G; @! S, F# O6 A! F9 d! D ~8 p: g$ _7 B$ p& C
JECFA关于二氧化钛(钛白粉)的结论
, E- e& _0 o# ^4 @! ]
0 a( `9 ~" U" C9 w摘要: 2006年JECFA关于二氧化钛的结论
7 P8 x/ b: [' X' KADI值:不作限制。) Y% A4 j+ K1 t! d
功能:着色剂' a9 y6 E7 _& ]4 u. c# `1 B
8 E7 O0 Z# V/ F3 J2 v0 G% D5 P
TITANIUM DIOXIDE
! d% g3 V) q5 E0 \" KPrepared at the 67th JECFA (2006) and published in FAO JECFA
; G. R9 l) v* b9 T; Z5 {2 |Monographs 3 (2006), superseding specifications prepared at the 63rd7 C) s; B" R9 M& h! ?8 D& H
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the+ l8 i, J8 Q1 k+ H- d" I8 J; ^
Combined Compendium of Food Additive Specifications, FAO JECFA
% ?6 |2 Q- z/ w9 w$ VMonographs 1 (2005). An ADI “not limited” was established at the 13th
0 m- a' z! S& X. {5 TJECFA (1969).
* @. U" r( T+ J) Z5 A# S8 CSYNONYMS
% y/ Y/ e- D* v4 A7 `9 j; _- dTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
5 _8 H" m' e8 o. iDEFINITION5 y# h; a/ g: u" d
Titanium dioxide is produced by either the sulfate or the chloride& s3 o4 H( m* H8 G& i
process. Processing conditions determine the form (anatase or rutile# _' |1 z" x! R# z# A
structure) of the final product.5 ~+ U2 \; v' ~- M ?
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
/ c' b( k {3 Y# s/ \or ilmenite and titanium slag. After a series of purification steps, the
$ I# o d# \* n! @! Nisolated titanium dioxide is finally washed with water, calcined, and5 ]! B% M* w# Q# G6 s2 I
micronized.) H9 x# X5 O4 L+ a4 z7 b. K V
In the chloride process, chlorine gas is reacted with a titaniumcontaining
- r! U) O. S2 ~- C! w# ?mineral under reducing conditions to form anhydrous! N k8 N2 l7 ]$ w
titanium tetrachloride, which is subsequently purified and converted to
' [4 Y7 } V6 v, n( I- C2 v6 H2 F( gtitanium dioxide either by direct thermal oxidation or by reaction with
r3 L' J/ D/ z/ j% s$ q2 s Isteam in the vapour phase. Alternatively, concentrated hydrochloric7 I1 p, L. x) {* w7 Z$ x, \; c
acid can be reacted with the titanium-containing mineral to form a
" ]) {6 N7 M; _8 \; Hsolution of titanium tetrachloride, which is then further purified and: g) a$ g3 e) B0 P+ R
converted to titanium dioxide by hydrolysis. The titanium dioxide is- \ @% S' u* i8 }2 K4 ]4 X- ~: L
filtered, washed, and calcined.
7 }0 r2 E! |& C' z+ a+ gCommercial titanium dioxide may be coated with small amounts of4 |% a' J, o6 M
alumina and/or silica to improve the technological properties of the
5 I, ^1 u4 N; l! Q5 l- Oproduct.
. i v* _9 W& U/ a+ I T! P2 r2 D cC.A.S. number 13463-67-7
+ m$ R$ J5 J( [Chemical formula TiO2
2 o& b! i5 ^( {Formula weight
9 `$ G! _2 H% o. m79.88
4 P. P. n: c& K5 U: c0 x( |Assay
# ]5 Z5 R& \) \. ~" i7 S4 mNot less than 99.0% on the dried basis (on an aluminium oxide and! V# [3 H7 \% h2 Q: _+ g
silicon dioxide-free basis)1 s- ]1 t9 @7 e" B b: T
DESCRIPTION2 v' q5 p0 k$ ^+ f; x; a
White to slightly coloured powder4 N% ?0 S2 [7 V' I6 B
FUNCTIONAL USES
0 N! `* k9 @3 d/ AColour3 i5 K) Y h; x
CHARACTERISTICS
/ S+ } F* L- p2 G+ NIDENTIFICATION
0 w. M% @% t/ e( T9 p+ K2 w/ O3 `8 }Solubility (Vol. 4)
$ T, t. J1 F5 _) T5 T5 aInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
8 T2 p- K* x8 ?* z; k; x4 c( Hsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
+ e9 c' u9 b. M, G5 N( [sulfuric acid.
4 k( Z3 J3 {# {& nColour reaction8 N) W# D$ b( B: z% C) A' e
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of; p- _6 X* t3 }# @2 _( ]: U6 g1 o
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with" X4 ?) Z8 V6 _: B* U$ J9 v; i
water and filter. To 5 ml of this clear filtrate, add a few drops of
' T# `! j$ R) P2 q+ z: }hydrogen peroxide; an orange-red colour appears immediately.# x: Y7 f* |/ X
PURITY0 K4 M$ Z6 B2 _3 r
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
% P' {6 x4 r% L, v# u! ?" tLoss on ignition (Vol. 4)
+ I X" K" ^/ K* { G0 }Not more than 1.0% (800o) on the dried basis
0 V* z6 w7 C, C" n5 y' o, L1 NAluminium oxide and/or
o* t7 C% k1 [silicon dioxide
S, k( j: A2 N8 VNot more than 2%, either singly or combined- n* w3 ?$ b+ V+ s+ |8 @
See descriptions under TESTS; W; Y! [# H5 W/ g3 q
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing2 L0 G. K5 L/ S/ O2 }
alumina or silica.
. N" v+ E a. Y( F7 c/ E6 DSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and. u% e0 f6 t0 F( G$ r+ g5 N+ ~' b
place on a steam bath for 30 min with occasional stirring. Filter- j; T9 t9 j% l6 [
through a Gooch crucible fitted with a glass fibre filter paper. Wash
: ^1 p6 x* E5 i* O+ S" @with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
: d, _& k( V& V0 r2 X& @4 c) H& c E) qcombined filtrate and washings to dryness, and ignite at a dull red( p5 N/ x8 }3 T+ ?9 C$ H/ W. s; Q" `
heat to constant weight.
3 p: h# F1 E8 B T1 {3 IWater-soluble matter, L0 z9 W/ z9 I- _
(Vol. 4)! O( p& h% e( R0 l9 ?
Not more than 0.5%
2 {) Y! C& ^. B0 Y4 f" qProceed as directed under acid-soluble substances (above), using
# C7 J7 C Z- ^2 Wwater in place of 0.5 N hydrochloric acid.
; [. [ q) X# B2 u W" J* rImpurities soluble in 0.5 N
6 z7 a$ ?( U* P8 H I$ v) lhydrochloric acid
/ N0 X& Q: w/ d/ DAntimony Not more than 2 mg/kg' D1 a7 y/ c6 O2 _, [) \, ?+ @
See description under TESTS
# n; H3 b7 U7 f/ f9 `2 [Arsenic Not more than 1 mg/kg) m% g) j! @( K8 v8 E
See description under TESTS2 p9 V+ i5 Q+ h& I9 ]( x
Cadmium Not more than 1 mg/kg1 v& \* c4 E# a
See description under TESTS
; G1 Y8 |9 F D% F1 ?9 @! vLead+ d8 a$ {4 p$ a, F% l
Not more than 10 mg/kg& y7 Z. k3 o$ _& k$ w% ^
See description under TESTS
; Q4 r6 H, N, A9 y. \4 ^Mercury (Vol. 4) Not more than 1 mg/kg, ~. @- C+ z) G, M$ I
Determine using the cold vapour atomic absorption technique. Select a
& {: q( A+ G3 S6 Xsample size appropriate to the specified level
# ]1 g. w2 t& c( G1 KTESTS0 a; ]0 k1 ?; ?$ y, x- F4 q
PURITY TESTS
& _# l$ L1 b* f+ G0 |; w% b! _Impurities soluble in 0.5 N. [/ A* e7 V a' E( i/ ? f; T
hydrochloric acid
0 W! [+ ^3 w; D" ?+ LAntimony, arsenic,
L+ Z4 _4 f) o4 t$ R4 Qcadmium and lead
. g. F, h# b. c6 [4 P; O(Vol.4)2 M6 V4 E4 {% U. s& j, F+ E; Y
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N0 f& K& ]; |- o
hydrochloric acid, cover with a watch glass, and heat to boiling on a+ K! C& C7 v4 u- Y! L
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml; h9 ?+ r" n( G; K6 {- E
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved* V9 _. U, N/ i. G4 P' R
material settles. Decant the supernatant extract through a Whatman
0 V$ I" _7 H: q5 V+ {No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml+ i0 A, d" Y1 E
volumetric flask and retaining as much as possible of the undissolved; ~, ~. m+ k2 \# _0 L
material in the centrifuge bottle. Add 10 ml of hot water to the original
5 N1 Z3 I6 \% k+ y& Nbeaker, washing off the watch glass with the water, and pour the: u& F0 F( f1 [5 S5 P& }: z$ U ]
contents into the centrifuge bottle. Form a slurry, using a glass stirring
/ W6 f8 \: o/ l1 Qrod, and centrifuge. Decant through the same filter paper, and collect7 ]; k* i0 [% C* {9 ]
the washings in the volumetric flask containing the initial extract.: }$ R e0 G5 c+ o- D& E
Repeat the entire washing process two more times. Finally, wash the
# e ^, i. S: X* s. ofilter paper with 10 to 15 ml of hot water. Cool the contents of the flask# Y q+ {/ _0 @4 g, t
to room temperature, dilute to volume with water, and mix.
: ?; h) U4 w8 y" I5 q- u* ~Determine antimony, cadmium, and lead using an AAS/ICP-AES7 F/ L# P5 _' X- z, T' p
technique appropriate to the specified level. Determine arsenic using the8 |8 t) w: m( u: i8 X8 L
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using, G4 z1 ^6 M/ a& I
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than" V0 b# D% s/ _3 |6 m
1 g. The selection of sample size and method of sample preparation
/ @* X; ^0 G) e7 Q x5 u+ jmay be based on the principles of the methods described in Volume 4." W$ b. R1 o3 S0 ]
Aluminium oxide Reagents and sample solutions, S7 h( o3 N6 I; J2 q' g2 o0 A
0.01 N Zinc Sulfate
# Z: P2 T2 ~0 H5 h, }Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
! {) g; g. E& d( T5 w" w! D+ ]make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
" B: J' _, e7 @of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of( n% K0 z7 f4 x6 M
concentrated hydrochloric acid, heating gently to effect solution, then4 w, {- I4 K# Q. U7 v3 Q3 X) b
transfer the solution into a 1000-ml volumetric flask, dilute to volume' E( C6 n3 G) Y% A/ W
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
$ Z |1 u- b7 Z Q. H# qml Erlenmeyer flask containing 90 ml of water and 3 ml of& v' y, ~4 i* |4 r/ a
concentrated hydrochloric acid, add 1 drop of methyl orange TS and2 M( I1 u5 J) F- P+ @) \
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
% \9 u B8 A( a/ Idropwise, ammonia solution (1 in 5) until the colour is just completely
* W$ P; G5 a. n1 T5 f! dchanged from red to orange-yellow. Then, add:( L% `. ~: b9 O& o4 |
(a): 10 ml of ammonium acetate buffer solution (77 g of
! O& ~6 e; t% ]% H+ e# qammonium acetate plus 10 ml of glacial acetic acid, dilute to
0 a q% d& h" q0 r/ y( h8 h. s1000 ml with water) and
9 R1 j* [6 }' g3 a! s6 {& y& T* q(b): 10 ml of diammonium hydrogen phosphate solution (150 g3 M4 G$ s/ A P9 w! F% e
of diammonium hydrogen phosphate in 700 ml of water,
6 w7 ?1 V; c# d6 Vadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
5 Z3 Z8 Y8 R( athen dilute to 1000 ml with water).
- h- j: k2 P( r' {/ r8 { |3 a' f7 YBoil the solution for 5 min, cool it quickly to room temperature in a! j5 z M4 h3 V; O2 }* [) B" i
stream of running water, add 3 drops of xylenol orange TS, and mix.
7 E- ~, u9 a0 C% oUsing the zinc sulfate solution as titrant, titrate the solution to the first
f: c! J( A5 j M& l/ ayellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
( d' [. E+ C6 h3 k2 y9 @& d8 ~This titration should be performed quickly near the end-point by
8 F( c" S7 T' c( K! q- y% L# cadding rapidly 0.2 ml increments of the titrant until the first colour9 t5 Q+ f) ?) E$ P
change occurs; although the colour will fade in 5-10 sec, it is the true/ N) d* ]/ D& l/ ]* L4 V
end-point. Failure to observe the first colour change will result in an
# q. h' L {3 M% c7 @/ S3 sincorrect titration. The fading end-point does not occur at the second
* i2 y( q9 g+ e0 send-point.)
+ ^, A6 W6 v3 Q# g1 L& lAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a. Z/ k' Q* x0 D( [, H( n6 ?
stream of running water. Titrate this solution, using the zinc sulfate# E7 R! S; v0 N& d( i
solution as titrant, to the same fugitive yellow-brown or pink end-point/ d* P) h y/ B, q! U
as described above.2 {( L. \1 J- I0 `& h3 D
Calculate the titre T of zinc sulfate solution by the formula:1 P4 J! p- \" F \9 S7 n
T = 18.896 W / V3 L( z: t g5 ~0 `- G
where! n% J' `/ d/ S& t% O ^3 H
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution# _ z3 u5 T8 q# x$ W0 ~# ?
W is the mass (g) of aluminium wire
; ]; U/ Q8 x0 K; d) O% oV is the ml of the zinc sulfate solution consumed in the, `" U" p% [0 Q# r8 d
second titration- F$ f$ [4 r2 p0 q+ B6 f
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
4 H: p' R" i" FR is the ratio of the formula weight of aluminium oxide to
+ E. ^% `9 y0 _0 j2 Y! p) H" o0 Bthat of elemental aluminium.2 ]* |1 O3 |6 p" Q3 M
Sample Solution A& s G5 L6 V/ R9 j/ H1 \
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
- |: C* k9 N& _ S( \# U/ N- Nglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
' q+ [; B, o" m: Y- S' q(Note: Do not use more sodium bisulfate than specified, as an excess
6 I, S; u2 v3 sconcentration of salt will interfere with the EDTA titration later on in the
& Z9 N# J" N8 a( Pprocedure.) Begin heating the flask at low heat on a hot plate, and
6 r6 [, t* }, n5 A; d& v9 Xthen gradually raise the temperature until full heat is reached.' l! A# V1 n& a- X! l b( P5 b: l! P Z
(Caution: perform this procedure in a well ventilated area. ) When
7 }3 e; Q& @9 [; x, I* F" S& }spattering has stopped and light fumes of SO3 appear, heat in the full3 R8 z& ?6 |- J- x6 E$ k7 D
flame of a Meeker burner, with the flask tilted so that the fusion of the
# {9 O9 N) u, S | z7 S$ usample and sodium bisulfate is concentrated at one end of the flask.
4 A' W+ d& z+ [- _- n* Z; g# H+ w3 @Swirl constantly until the melt is clear (except for silica content), but8 o3 \5 d& b4 O. W* ]- U( @) G
guard against prolonged heating to avoid precipitation of titanium8 t9 q; F' t9 S' Q) R5 H) b1 E
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until- R( w Y# y& b. ?4 F( _9 G* ?' {
the mass has dissolved and a clear solution results. Cool, and dilute to# W# O2 l" P% T
120 ml with water. Introduce a magnetic stir bar into the flask./ f: T0 N3 z# e. ^
Sample Solution B4 H& i* f0 z- _1 j& H
Prepare 200 ml of an approximately 6.25 M solution of sodium3 X( E% q O( |/ w. h9 v4 Z
hydroxide. Add 65 ml of this solution to Sample Solution A, while
# J: O1 |0 R7 b- ]% E' ]1 istirring with the magnetic stirrer; pour the remaining 135 ml of the
" ` [ ^1 h3 L6 ^( ~1 }alkali solution into a 500-ml volumetric flask.
1 |) R# {4 d' _Slowly, with constant stirring, add the sample mixture to the alkali
% u- G" H9 c5 w! M2 c, @9 \solution in the 500-ml volumetric flask; dilute to volume with water,
2 j5 Y" N: {" _ M! tand mix. (Note: If the procedure is delayed at this point for more than
+ B2 m. ~; Z& K6 d7 X2 hours, store the contents of the volumetric flask in a polyethylene
. L" w" F# G% H x% _& Y8 }5 Ebottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),( T% k V+ w4 I/ {7 e
then filter the supernatant liquid through a very fine filter paper. Label
& c# r c* U( Wthe filtrate Sample Solution B.! R6 }' R, \4 ~% t5 C6 C
Sample Solution C
. N' \- @7 _, ~& U! J( ATransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer; X, D; A* z5 r$ o. Y
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
. A1 j. Q, ^; |9 msolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02" X- K9 s+ N' M# N2 j0 {
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
' E ~& m# r0 b. X; t. Y; Lknown, calculate the optimum volume of EDTA solution to be added7 j3 p% k6 e/ k" ?7 F$ m
by the formula: (4 x % Al2O3) + 5.]
4 v( t8 ?( t5 ~4 K; ^0 Y! }Add, dropwise, ammonia solution (1 in 5) until the colour is just
/ N2 x" r. v% c0 bcompletely changed from red to orange-yellow. Then add10 ml each
+ ` j, \+ t9 [: n6 ^of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to6 `% o( L8 M. z- c) g5 k
room temperature in a stream of running water, add 3 drops of xylenol
% V! `- r4 m! e. ^0 forange TS, and mix. If the solution is purple, yellow-brown, or pink,
7 ~% W! [% I& s* _ \" w0 Pbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
+ z! k* a# n6 fpH, a pink colour indicates that not enough of the EDTA solution has
9 `. C& n8 Q2 K0 ]2 O& _# Zbeen added, in which case, discard the solution and repeat this
& |# Y; }, d0 k0 W! Vprocedure with another 100 ml of Sample Solution B, using 50 ml,
, ?( U3 B! z Frather than 25 ml, of 0.02 M disodium EDTA.
7 R3 b* H2 r+ |2 b, c6 R/ l% W, NProcedure
2 w. [( ^) h. N. M4 D2 JUsing the standardized zinc sulfate solution as titrant, titrate Sample
/ c9 o, @1 U) b! C$ V3 }2 ^Solution C to the first yellow-brown or pink end-point that persists for* q) Y* {& `5 U
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
2 ~' e Q0 Z7 G9 D; A' s7 ~titration should require more than 8 ml of titrant, but for more accurate
# z* p0 b/ W5 g% z! E* Qwork a titration of 10-15 ml is desirable. w& n& t8 o3 ]9 s2 L. l
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
; v* V$ |; X4 v% xmin, and cool in a stream of running water. Titrate this solution, using1 m3 |6 W4 G5 |* Z i8 I' \
the standardized zinc sulfate solution as titrant, to the same fugitive) U/ B. @8 n0 j. `- P
yellow-brown or pink end-point as described above.+ j, g! T; T4 F) w+ _8 z. `
Calculation:7 \" ~+ [/ A( e+ d1 ]& X2 v' C
Calculate the percentage of aluminium oxide (Al2O3) in the sample
7 H# B! S! ?* P' ~ F4 J; {taken by the formula:
; Q# P( I1 j& {% Al2O3 = 100 × (0.005VT)/S
: |: q6 {9 W/ L: _0 Z9 Mwhere H2 a, \- l8 o- _+ ^# r! S
V is the number of ml of 0.01 N zinc sulfate consumed in
& s7 n+ I2 H9 Y8 I3 Y( C$ ithe second titration,
( T! Z# \4 S L: L5 u% m3 VT is the titre of the zinc sulfate solution,
: y/ s* O: K: r; Q3 ]& Q2 l; cS is the mass (g) of the sample taken, and5 Q/ I6 V4 M' P: \1 P
0.005 = 500 ml / (1000mg/g × 100 ml).
0 T; h7 P+ }# |; u2 O% lSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica. ? i- c }! x: J
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).3 U+ W, s' S9 \# i$ M" e: o( U; ~ l
Heat gently over a Meeker burner, while swirling the flask, until
! }, ~0 i8 C( zdecomposition and fusion are complete and the melt is clear, except
4 C8 R/ H5 n# V8 N6 q. Bfor the silica content, and then cool. (Caution: Do not overheat the3 G% Q2 r; U+ P9 f! r% k$ L
contents of the flask at the beginning, and heat cautiously during) B, M7 }) X7 X
fusion to avoid spattering.)* i7 f! F) @0 j. N+ [
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
4 G; X( s' }/ V3 Ecarefully and slowly until the melt is dissolved. Cool, and carefully add4 w6 M! j: ~+ s# `. S! C
150 ml of water by pouring very small portions down the sides of the# \* P& \% w! W0 Z$ }6 W
flask, with frequent swirling to avoid over-heating and spattering. Allow- b% s# `3 [1 D2 N. d8 ]
the contents of the flask to cool, and filter through fine ashless filter' d5 |% H) o+ m% p5 p3 H" b6 L7 k2 M" d
paper, using a 60 degree gravity funnel. Rinse out all the silica from9 x0 q( z1 }/ {/ ?3 |, s
the flask onto the filter paper with sulfuric acid solution (1 in 10).
9 x# z" S7 j! j+ Z& eTransfer the filter paper and its contents into a platinum crucible, dry in) Z6 k9 a# I; r1 i! S: I
an oven at 1200, and heat the partly covered crucible over a Bunsen
3 d* o* f2 \5 z* @burner. To prevent flaming of the filter paper, first heat the cover from# c* E/ @# y5 r; `! S" [
above, and then the crucible from below.
/ Z1 _2 [" `- [. U% u5 g0 dWhen the filter paper is consumed, transfer the crucible to a muffle9 J' J- ]- I; N9 z
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and8 Q8 I' u* `3 T& Y, H7 q+ y$ L
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
$ j! H7 e, P5 i' x) q9 shydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
( U) D1 O) U' Q* a+ C) X& Non a low-heat hot plate (to remove the HF) and then over a Bunsen
n) T8 l5 F. `; ]burner (to remove the H2SO4). Take precautions to avoid spattering,
' h+ \0 r2 s2 B: v8 N% b+ _, eespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
7 m/ L, m7 o3 a3 O. {9 ^3 @7 ^desiccator, and weigh again. Record the difference between the two4 R$ D1 X* z O9 F7 ^8 A
weights as the content of SiO2 in the sample.' T& [3 \" Q9 H& ~
METHOD OF ASSAY7 _* ?( h- }; {( V
Accurately weigh about 150 mg of the sample, previously dried at 105o
' _, j. }! M5 X0 d3 t6 J% Zfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
. m+ J$ X+ s5 w$ w5 X* A3 M" Band shake until a homogeneous, milky suspension is obtained. Add 30. H- _7 p3 k1 }7 L6 V
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
2 R% ~9 v5 d, xheat gently, then heat strongly until a clear solution is obtained. Cool,) S9 Y% n. K1 r3 O: m
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
& {" [8 P% f, V: `acid, and stir. Add 3 g of aluminium metal, and immediately insert a1 K$ v' p- l8 t- M- y+ ?& e
rubber stopper fitted with a U-shaped glass tube while immersing the
+ o6 c5 t$ ~* w5 k5 J! R$ qother end of the U-tube into a saturated solution of sodium9 ^2 X5 D& o! {9 X5 V: Z( c$ ?
bicarbonate contained in a 500-ml wide-mouth bottle, and generate6 b& X% ~- u! r- B5 a. t
hydrogen. Allow to stand for a few minutes after the aluminium metal
+ L1 @* r1 U6 lhas dissolved completely to produce a transparent purple solution.# O9 b, r8 h+ z) c6 r" ^! L7 h y
Cool to below 50o in running water, and remove the rubber stopper: f; r; M" D( E( Y# s
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate. s( l7 ?2 K1 P) }
solution as an indicator, and immediately titrate with 0.2 N ferric
U+ W0 m' h# W) m0 Kammonium sulfate until a faint brown colour that persists for 30$ h2 }- z! G( n$ `
seconds is obtained. Perform a blank determination and make any( l3 U/ j# U$ }% b1 F, `5 Z1 S
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is3 T( D. N( [) g+ Z, U2 n
equivalent to 7.990 mg of TiO2.
; b X3 K. q3 X! }% N H |
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