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二氧化钛(钛白粉)
二氧化钛(钛白粉)
1 S7 z( L: v- p2 a1 `
8 x$ W* K+ \4 T0 N; R7 KJECFA关于二氧化钛(钛白粉)的结论) @4 v; A1 k" E( x( b+ ^; y
' Q9 F( k( T; c, K/ T
摘要: 2006年JECFA关于二氧化钛的结论! l) E5 f6 k7 Y7 {" g o2 F. G+ F
ADI值:不作限制。
1 |3 q) m* u) J4 r* S, ]0 K+ k功能:着色剂* ]. Q9 ?. P( K9 U( Q g: ]. j
- m+ p9 J: [' ^TITANIUM DIOXIDE2 T9 O# `) D- Y/ N$ }
Prepared at the 67th JECFA (2006) and published in FAO JECFA' @. _% X( a4 F: g7 o _& ^8 o
Monographs 3 (2006), superseding specifications prepared at the 63rd
: k% J1 e, h+ B) ^9 F9 cJECFA (2004) and published in FNP 52 Add 12 (2004) and in the b9 M0 B. Z) x' S/ o
Combined Compendium of Food Additive Specifications, FAO JECFA
/ _# M$ i; x' c6 @' cMonographs 1 (2005). An ADI “not limited” was established at the 13th
- @6 g2 a# V- uJECFA (1969).
5 N+ U2 z Z2 G0 l0 s2 F# f% G- @SYNONYMS
3 S& i D8 v; q9 qTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1710 f% W' z* ] W# o/ f
DEFINITION
* W/ p$ c! z$ s" M6 LTitanium dioxide is produced by either the sulfate or the chloride
+ ]( n; |' m, yprocess. Processing conditions determine the form (anatase or rutile
5 S8 B! |/ }* o! p% q; Ystructure) of the final product.5 X, J* u, Z: c2 ~/ p
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
/ m6 j, E, g: U" g8 Y1 zor ilmenite and titanium slag. After a series of purification steps, the$ j' f9 _( r, m* |8 t
isolated titanium dioxide is finally washed with water, calcined, and& q3 ?: x6 K) o; U
micronized.
2 W0 {, ~& f* k' _8 S( f4 E! QIn the chloride process, chlorine gas is reacted with a titaniumcontaining
5 u! K ^; B% [4 r' tmineral under reducing conditions to form anhydrous) ^( o9 H: Q( S6 A; y. M
titanium tetrachloride, which is subsequently purified and converted to
6 ~5 T8 F$ P' R% y5 ^titanium dioxide either by direct thermal oxidation or by reaction with
# H+ `+ L- _1 a' e% Psteam in the vapour phase. Alternatively, concentrated hydrochloric/ `- L7 T/ k6 L2 N, }) y9 M
acid can be reacted with the titanium-containing mineral to form a1 O5 u6 H y: c7 x1 j, Z
solution of titanium tetrachloride, which is then further purified and
' M, v/ T: @3 v) x8 r) Yconverted to titanium dioxide by hydrolysis. The titanium dioxide is/ O/ D- r! r( r6 Y' `3 [6 P
filtered, washed, and calcined.& B$ d& K7 H4 E f
Commercial titanium dioxide may be coated with small amounts of
7 Q5 P. x1 I1 K6 L- kalumina and/or silica to improve the technological properties of the
6 M% \4 a! V$ t' p2 {# O, o9 {product.; I5 {0 [6 N$ I$ I
C.A.S. number 13463-67-7
8 e8 u6 w* L1 G& X0 {Chemical formula TiO2
) p9 V5 |9 H* }6 h1 J2 rFormula weight
3 ~( A1 E, s) Q8 b3 d79.88
2 z2 ?" ]! c2 T1 gAssay
+ G+ s( J$ {% j6 L, xNot less than 99.0% on the dried basis (on an aluminium oxide and
, h" h( D q) H* I# g# Z! Qsilicon dioxide-free basis)
+ k+ i( Q/ U0 b2 o- \DESCRIPTION. V/ s) U7 s5 o: A7 W" g. }0 D' R4 V
White to slightly coloured powder
+ I/ j! y' n3 \FUNCTIONAL USES
9 n( b2 l0 K) f Z; B+ YColour
" D# Q# R# O. c0 M2 ACHARACTERISTICS
! u$ G; f, G( CIDENTIFICATION
* q. e0 f6 U9 x, O1 N' jSolubility (Vol. 4)8 t% l) h, c7 x
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic, b) F& Z' V- P$ T# k
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
$ Y+ g3 w8 \, S+ s2 `7 v! ssulfuric acid. { A/ b# `! J! C
Colour reaction( g0 i/ W" z5 s4 N9 ?; A3 B
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of+ ? I: [7 j U+ x/ \' ]6 b3 K: Q" \
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with- r/ g* X0 Q6 i7 U. k" I
water and filter. To 5 ml of this clear filtrate, add a few drops of
9 @1 r u T9 rhydrogen peroxide; an orange-red colour appears immediately.
/ Z0 s1 G8 H5 J. W; X& vPURITY
4 Z4 H5 @0 X# J/ l4 q2 rLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
8 J7 O% B; _) J+ q% X& |* [Loss on ignition (Vol. 4); G5 Z+ U% i+ U5 G
Not more than 1.0% (800o) on the dried basis. m. {1 C, t# x# I' O4 _0 i* E
Aluminium oxide and/or
1 \) |4 \+ s8 p3 y' c6 Y7 ysilicon dioxide
6 T7 o& j: |) _8 z1 W. c, O0 `Not more than 2%, either singly or combined
+ R; y( w! ~1 R# o% g. w5 LSee descriptions under TESTS
, s- t' u+ h/ ?' @: g, EAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
9 M4 f8 z* ^2 ~4 C4 B3 W, ?+ Jalumina or silica.# ^6 v6 V8 j# @3 ]
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
; `% R1 Z( V% J9 F: [place on a steam bath for 30 min with occasional stirring. Filter) z) X i1 k6 }, ]& i$ I
through a Gooch crucible fitted with a glass fibre filter paper. Wash w- x! Z6 K1 [! v
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the0 |: N5 f0 o' \+ ?% q5 ]
combined filtrate and washings to dryness, and ignite at a dull red
: v! ^1 L9 f) F- l$ mheat to constant weight.
- W+ w7 A! S* b5 T+ E- j5 }Water-soluble matter
2 {% X, S8 V! z, f% d(Vol. 4)
" e& s4 B8 n* u+ e, h* LNot more than 0.5%
1 o' s! p1 s/ m9 \# hProceed as directed under acid-soluble substances (above), using
: ~% Q0 R* R: R" y" s0 N0 S- g' ewater in place of 0.5 N hydrochloric acid.! `+ g% }5 s9 s1 s4 C$ v
Impurities soluble in 0.5 N
7 x- [7 o4 v6 i" Zhydrochloric acid
$ y. A6 [. i$ t+ q! y$ qAntimony Not more than 2 mg/kg
( @+ h' O# J5 b7 j$ O- I0 W9 PSee description under TESTS
; g: e* u# b/ L; kArsenic Not more than 1 mg/kg
/ N |4 k9 W* j& g1 zSee description under TESTS3 r7 G( d8 a- p5 n( c* k' N7 F& @$ [
Cadmium Not more than 1 mg/kg
8 _- f9 m( R$ O! P0 NSee description under TESTS8 R; x2 G+ x- g% S
Lead
3 Z! a/ c. Q4 z* S1 I7 M. T) TNot more than 10 mg/kg
& W/ V0 [/ Q4 v, q* I- H* SSee description under TESTS
2 H- G8 g7 O7 e% RMercury (Vol. 4) Not more than 1 mg/kg* p% F. e- B' q' p' B: z% |4 y3 ?
Determine using the cold vapour atomic absorption technique. Select a
9 B2 M B' n, f) @7 ^sample size appropriate to the specified level) e L [7 @: u7 m; E9 Y
TESTS
- Q" d' Q9 r% B* ?0 i: Z1 N3 ~PURITY TESTS" y* X9 B- o$ p' i. W
Impurities soluble in 0.5 N
. X( {4 `/ v, [1 Z( T9 F Bhydrochloric acid; }, u, v; D( Z1 p- s
Antimony, arsenic,
$ E- k% b' g7 j ^# u- tcadmium and lead
8 O7 e; K, R+ o6 ](Vol.4)( F: H. y5 b8 W, F& i3 Y, G$ |
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
5 M! x, P+ v! E& ]6 j- S. Whydrochloric acid, cover with a watch glass, and heat to boiling on a8 a) E) p6 P, h |$ m
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
# [4 ]9 p, ?& k( Hcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved$ K% j- _ R- i3 h& E1 M3 u
material settles. Decant the supernatant extract through a Whatman
9 O: Z( ^6 L& ]* e" JNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
5 F& K2 C: K! O3 _ Uvolumetric flask and retaining as much as possible of the undissolved2 T3 U, c6 x+ d1 o: Y
material in the centrifuge bottle. Add 10 ml of hot water to the original" e* v" k8 k% {% C. B; t% t; Y* L+ U+ E
beaker, washing off the watch glass with the water, and pour the
* i" u0 f9 ?8 X3 h$ dcontents into the centrifuge bottle. Form a slurry, using a glass stirring
" \2 g' {% m& \% w! e3 c3 J0 srod, and centrifuge. Decant through the same filter paper, and collect; R9 ^- t4 M" L4 U, t% M+ l
the washings in the volumetric flask containing the initial extract.
" a Z! E, x) h. v2 ?9 ^Repeat the entire washing process two more times. Finally, wash the
& K9 ]6 E% ~; Tfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
6 O0 N+ \# I# \0 o- }( rto room temperature, dilute to volume with water, and mix.
. U# G0 { N( y1 z0 ^' [* g! HDetermine antimony, cadmium, and lead using an AAS/ICP-AES8 F+ @2 L, t& p* J& X L
technique appropriate to the specified level. Determine arsenic using the
1 d; ~! C; L, n; r. l$ j& c C/ s IICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
r9 P5 E( F8 a+ I! z5 x: lMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than$ |$ W% U% w# [( i0 J2 K% j* D& w9 N
1 g. The selection of sample size and method of sample preparation
, A/ W' t( a" Q& u, Cmay be based on the principles of the methods described in Volume 4.
3 G! G2 s7 R; n' W7 UAluminium oxide Reagents and sample solutions$ a+ \7 B% L5 i' a6 {3 U* C
0.01 N Zinc Sulfate" u; @) y9 m/ ^; B
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
- o, _% ^' l- g6 d8 [make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
- B6 O& u: e+ Z# yof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of6 U2 v- T7 ~1 w/ U7 }4 U; G
concentrated hydrochloric acid, heating gently to effect solution, then0 O1 ~, @% D! J8 U4 J( m& q. E
transfer the solution into a 1000-ml volumetric flask, dilute to volume
% J! n; o& Q' }3 Bwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
3 i/ A# r& x D z% A) gml Erlenmeyer flask containing 90 ml of water and 3 ml of( C( ^" @3 D9 R6 I4 H4 Z( \0 r
concentrated hydrochloric acid, add 1 drop of methyl orange TS and5 t8 t, Z- n) a/ j; E3 U3 P
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
8 l# P# ?8 w" s @) j. ~dropwise, ammonia solution (1 in 5) until the colour is just completely) { A' A. K1 G
changed from red to orange-yellow. Then, add:
3 F6 ?; ?$ d$ W& ]* R(a): 10 ml of ammonium acetate buffer solution (77 g of
* U1 J. L- }; v0 [+ hammonium acetate plus 10 ml of glacial acetic acid, dilute to
* {8 o( i! _( Z9 I1000 ml with water) and
5 x; y/ @% W3 m1 I(b): 10 ml of diammonium hydrogen phosphate solution (150 g R* [9 [0 o. l! l: `$ [# m
of diammonium hydrogen phosphate in 700 ml of water,3 s% r) N' r3 d3 a5 ^' y/ o( N. N5 Y: |
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
" s$ {, u+ D5 P& I0 @then dilute to 1000 ml with water).
+ P# Y) ^ N- i! UBoil the solution for 5 min, cool it quickly to room temperature in a' I' e; G+ a. N+ r4 `' C
stream of running water, add 3 drops of xylenol orange TS, and mix.: m0 d4 B0 d. ^( W. ^9 l& Z
Using the zinc sulfate solution as titrant, titrate the solution to the first
6 F* J5 }' I% a. g, D" Ryellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
; w0 W# J! p9 t& M1 x, cThis titration should be performed quickly near the end-point by
8 o/ [# P3 n, W" x+ L8 Dadding rapidly 0.2 ml increments of the titrant until the first colour
Q3 I0 d% m! j- X% H3 F {. h3 tchange occurs; although the colour will fade in 5-10 sec, it is the true" C; ?5 z; ]/ }* t6 `& j
end-point. Failure to observe the first colour change will result in an/ E5 [; M* e" ^7 W$ Y( ]6 M- B$ `
incorrect titration. The fading end-point does not occur at the second! q3 I5 G0 y" e, d
end-point.)
q& g& ~* _3 f) K) f0 V0 L) w; YAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a# U/ B4 y! H. l- y( X4 X5 d
stream of running water. Titrate this solution, using the zinc sulfate
! J# Q4 v; I* b9 ^; c7 G3 zsolution as titrant, to the same fugitive yellow-brown or pink end-point' x, l, P: K6 }% H3 o- L2 ?
as described above.4 k2 o) t6 N% ^3 q/ z! |4 J+ {1 a
Calculate the titre T of zinc sulfate solution by the formula:
9 \/ g$ A" Z1 @) I" ?* ]T = 18.896 W / V
! _( ^$ S" p" y2 d4 Vwhere
8 j; @- ]# E5 P9 e$ nT is the mass (mg) of Al2O3 per ml of zinc sulfate solution$ Q- D& ~- q _: U; a. \5 H( ]# e" g+ x
W is the mass (g) of aluminium wire3 q; o( d; }6 w& Y& i
V is the ml of the zinc sulfate solution consumed in the7 @% q( H2 r# a# y u2 I9 G4 k* B
second titration
0 |+ P: Q8 n3 f/ w, H$ d18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
' y' y6 [ ^5 B9 Y& Q& aR is the ratio of the formula weight of aluminium oxide to
/ Q4 ^; B, y: B" R( Zthat of elemental aluminium.
$ z5 D/ L2 I6 U+ ^( rSample Solution A
& k$ ~2 D6 D9 \. T3 OAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica; P1 V+ B, c- R, v
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
% @( n/ o" r9 k n(Note: Do not use more sodium bisulfate than specified, as an excess
2 k$ E* a, {0 \3 {, \concentration of salt will interfere with the EDTA titration later on in the
( K3 }" g: V5 H* n+ b: f, o- S; v' xprocedure.) Begin heating the flask at low heat on a hot plate, and' k) i1 C F/ _( `$ l
then gradually raise the temperature until full heat is reached.: [* ^' y( A4 n
(Caution: perform this procedure in a well ventilated area. ) When
3 T, X2 Y: f2 k3 m- V/ J% uspattering has stopped and light fumes of SO3 appear, heat in the full+ g, r& G7 d& b6 f+ F
flame of a Meeker burner, with the flask tilted so that the fusion of the: N6 J; \- g; e& C) W5 R* Y
sample and sodium bisulfate is concentrated at one end of the flask./ W, R: Q( _% ? }8 G( N
Swirl constantly until the melt is clear (except for silica content), but
! B/ E a: B8 e# a0 o. Yguard against prolonged heating to avoid precipitation of titanium
/ b- s' c) ^" u% cdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until* ?* U/ @; `; t' J
the mass has dissolved and a clear solution results. Cool, and dilute to1 Z u' v/ n& n1 a
120 ml with water. Introduce a magnetic stir bar into the flask.
R; r8 F/ j1 p" kSample Solution B
6 U6 e6 q( S2 M, X8 pPrepare 200 ml of an approximately 6.25 M solution of sodium7 |2 |8 j4 P& Y& Q$ v% P
hydroxide. Add 65 ml of this solution to Sample Solution A, while& @6 y3 _% o1 D2 o
stirring with the magnetic stirrer; pour the remaining 135 ml of the
! u9 M: f Q% E: ?; oalkali solution into a 500-ml volumetric flask.
* z( N3 l2 y) d. F- v- y9 j8 vSlowly, with constant stirring, add the sample mixture to the alkali$ @8 ?* a- P. l, p
solution in the 500-ml volumetric flask; dilute to volume with water,
1 T: G( y5 c% x$ Kand mix. (Note: If the procedure is delayed at this point for more than' F/ C0 J5 }: N
2 hours, store the contents of the volumetric flask in a polyethylene+ B' W, `3 j5 K6 Q& i0 w& G
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),0 ^, d, p6 M- _
then filter the supernatant liquid through a very fine filter paper. Label- ^/ F* j" w; D; o5 q; H2 \& L; Z
the filtrate Sample Solution B.0 }. P! o" |" B+ ^3 I" @+ _
Sample Solution C, X3 i1 M; n: f" F0 B1 W7 k
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
4 \8 q4 M+ x; X/ Pflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid+ F( `9 i/ O+ d8 t
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
0 V0 I, |, z/ E6 M- {M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is5 J2 H9 B3 A# Z
known, calculate the optimum volume of EDTA solution to be added
# B! O) r7 Y$ P9 `& F- Cby the formula: (4 x % Al2O3) + 5.]2 [! k' T+ R$ Y7 w' k4 i
Add, dropwise, ammonia solution (1 in 5) until the colour is just
" ~* N4 i) G# tcompletely changed from red to orange-yellow. Then add10 ml each
$ B, R9 X2 l! q3 j& B; F9 qof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to" q" l: o3 h3 O% @; Q# x
room temperature in a stream of running water, add 3 drops of xylenol
8 A$ U8 X& b* W# g( b; E' [2 ]' zorange TS, and mix. If the solution is purple, yellow-brown, or pink,
2 Y! d( a& C& K3 W9 ?5 R: p' E; fbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired( |$ F, u, p7 Q @ K
pH, a pink colour indicates that not enough of the EDTA solution has
2 `& O% R; P+ X9 Jbeen added, in which case, discard the solution and repeat this( H8 P' \; ]1 V) v: J# @
procedure with another 100 ml of Sample Solution B, using 50 ml,3 L/ N/ w8 M' T6 p) o. G4 d
rather than 25 ml, of 0.02 M disodium EDTA.
! d) H0 c2 ?9 f4 CProcedure
/ i$ g# J2 J. H$ u% Q4 \2 @Using the standardized zinc sulfate solution as titrant, titrate Sample
/ g& J, W4 @' c; D0 D+ KSolution C to the first yellow-brown or pink end-point that persists for3 u' k, n* L4 h* Z
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first7 d# L! G+ m9 ?8 ~
titration should require more than 8 ml of titrant, but for more accurate
9 K9 A* N7 N/ m0 Hwork a titration of 10-15 ml is desirable.0 W& b. X8 A, ?: i2 p. n3 v
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5# r7 U, y3 B3 w0 `, d: M. u
min, and cool in a stream of running water. Titrate this solution, using
& Q; H- M$ ^" Pthe standardized zinc sulfate solution as titrant, to the same fugitive
9 g/ N; B3 }) H( G6 v# `0 Uyellow-brown or pink end-point as described above.
( N, a' G/ v; G8 d: L- N% VCalculation:5 L b$ ~5 {, k/ T2 r( ]0 O
Calculate the percentage of aluminium oxide (Al2O3) in the sample
9 T, x3 t# T. r9 f1 Itaken by the formula:
0 t8 l9 [% |8 x9 Y! O6 z% Al2O3 = 100 × (0.005VT)/S
, S# K9 g3 c+ s( a, r4 o+ fwhere
5 g# e. I3 l2 UV is the number of ml of 0.01 N zinc sulfate consumed in- ?6 _" z% w, @) h! R$ z6 X& K
the second titration,
0 f J+ ?1 h. s2 D, A) a. }" v9 IT is the titre of the zinc sulfate solution,$ Q" ?! X, p/ ?4 ~; K. A3 D
S is the mass (g) of the sample taken, and
! z. } V7 V0 |! y: g0.005 = 500 ml / (1000mg/g × 100 ml).( N" C! K* a3 _
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica' K: @. `$ D9 `, _4 V) h* b
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
& ` B: ^1 ~/ |' ^Heat gently over a Meeker burner, while swirling the flask, until. g- F+ Y1 a+ E
decomposition and fusion are complete and the melt is clear, except R4 @ g6 ?7 p
for the silica content, and then cool. (Caution: Do not overheat the3 r& w/ k1 _+ |0 {* q) k
contents of the flask at the beginning, and heat cautiously during
0 q! K& I+ X4 r2 Nfusion to avoid spattering.)/ r; z: I' J# v' i
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
! Q/ r; T+ Y6 X9 V5 ycarefully and slowly until the melt is dissolved. Cool, and carefully add( |- E. [, T: {4 \5 _
150 ml of water by pouring very small portions down the sides of the
: c+ U: Q- h+ V( W) q" j* lflask, with frequent swirling to avoid over-heating and spattering. Allow
) `7 T! o: e Pthe contents of the flask to cool, and filter through fine ashless filter" k% S, a! H/ }* m7 S, t* Q' x4 K9 T
paper, using a 60 degree gravity funnel. Rinse out all the silica from; P o8 Q& y, D* s9 n
the flask onto the filter paper with sulfuric acid solution (1 in 10).
0 }$ R5 y9 _! Q" l1 C" `: y( H/ |Transfer the filter paper and its contents into a platinum crucible, dry in
4 H* W0 e! c% m2 y$ a# W$ t; nan oven at 1200, and heat the partly covered crucible over a Bunsen
3 Q& ~6 z1 o }; Q& r) sburner. To prevent flaming of the filter paper, first heat the cover from* d, ?3 F$ ~2 u, ?' _* f' a
above, and then the crucible from below. G% f9 K- |8 E2 z/ r v2 q$ Y
When the filter paper is consumed, transfer the crucible to a muffle
! @ ?' C6 Z7 s t2 v0 [* wfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and3 g% w. v/ D6 _
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated8 O R5 h) }6 M( o# E0 z7 {4 C
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first9 ^- w+ O {& P% W
on a low-heat hot plate (to remove the HF) and then over a Bunsen
Y/ k x2 M& E, aburner (to remove the H2SO4). Take precautions to avoid spattering,# T( f/ S4 M4 z5 e+ {' b
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
/ t( b. d- ?! ^8 Sdesiccator, and weigh again. Record the difference between the two+ \4 ?$ }4 O: U
weights as the content of SiO2 in the sample." m2 A* m+ ]. k1 q' L
METHOD OF ASSAY
6 `& i3 F. r0 e+ Z' N2 j: VAccurately weigh about 150 mg of the sample, previously dried at 105o' ]3 K. u6 C2 F) k
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water3 ^ g9 e4 j$ B0 O
and shake until a homogeneous, milky suspension is obtained. Add 30
) L; ~4 C& g* ~, Sml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
3 E$ h/ H" }. O& p2 f. ^- Aheat gently, then heat strongly until a clear solution is obtained. Cool,) A- o" j& Q, u0 G1 V
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric' A! ?; o9 B; Y1 L
acid, and stir. Add 3 g of aluminium metal, and immediately insert a1 i+ Q$ {: Q# O2 Q0 Q1 m( v& j6 a9 X* b
rubber stopper fitted with a U-shaped glass tube while immersing the
6 I, o$ A$ M) p1 k: \6 J, I+ }other end of the U-tube into a saturated solution of sodium
5 _( ]7 K3 m! Bbicarbonate contained in a 500-ml wide-mouth bottle, and generate
Y/ K7 X6 I' X% d& P& i ]hydrogen. Allow to stand for a few minutes after the aluminium metal0 `9 ~, i0 k. _+ P
has dissolved completely to produce a transparent purple solution.$ F, S/ I" c. |4 Z
Cool to below 50o in running water, and remove the rubber stopper7 [8 I8 g+ x( h1 f' f
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate/ J( r+ \3 [3 O5 k6 d
solution as an indicator, and immediately titrate with 0.2 N ferric2 G# j2 }/ ~' B. [
ammonium sulfate until a faint brown colour that persists for 30
! m0 j& g2 U, t7 ~) J, kseconds is obtained. Perform a blank determination and make any
! V, o, w# U3 ]' @necessary correction. Each ml of 0.2 N ferric ammonium sulfate is5 b. g! U$ |6 w# v
equivalent to 7.990 mg of TiO2.$ V3 d+ O# q1 @) V
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