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二氧化钛(钛白粉)
二氧化钛(钛白粉)" B1 [) V3 T+ S3 d
$ g; A- ?" ^. K7 a. t
JECFA关于二氧化钛(钛白粉)的结论3 s% D: ^! D- ~ R4 x. k& }
2 `( J1 H8 n$ {7 k7 v摘要: 2006年JECFA关于二氧化钛的结论
+ C- O0 x5 v. }9 |5 U8 y4 g6 B, sADI值:不作限制。. N: z6 k9 V6 Y7 a
功能:着色剂
8 W, v5 Z5 ]- X, P! ]9 `) G: z! h x
TITANIUM DIOXIDE1 G% `9 x' |$ _ P+ R3 R* D/ P1 B ~
Prepared at the 67th JECFA (2006) and published in FAO JECFA @, l0 C [& w; j6 G% e- b
Monographs 3 (2006), superseding specifications prepared at the 63rd
/ u. z0 ?2 u0 I1 J- Z7 j; Z! Z) _JECFA (2004) and published in FNP 52 Add 12 (2004) and in the. M6 Q3 _+ z; |
Combined Compendium of Food Additive Specifications, FAO JECFA
, x* s5 i0 t4 uMonographs 1 (2005). An ADI “not limited” was established at the 13th
1 z2 o5 @/ }- r+ aJECFA (1969).
3 h4 Q! r. N# K. QSYNONYMS
9 D+ t6 c. j5 P$ b/ X# e) }/ MTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1714 m6 j \: K% W; K, V1 c: `2 I
DEFINITION, C5 o' L5 q. ~2 F
Titanium dioxide is produced by either the sulfate or the chloride. s9 W7 A2 g6 V: A4 q6 }
process. Processing conditions determine the form (anatase or rutile
7 K7 R4 |9 `1 \! Astructure) of the final product.
: O6 |# R: t" O5 O" V- iIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)1 {' w: p$ ?- G# ?
or ilmenite and titanium slag. After a series of purification steps, the" r* A$ q) N: w/ G) b' e$ G/ [
isolated titanium dioxide is finally washed with water, calcined, and8 h, K8 ?; ^7 a* V/ @0 x0 [: X
micronized.
8 }7 M% b6 Z1 NIn the chloride process, chlorine gas is reacted with a titaniumcontaining
: Y- m, U9 T- R' P6 H' Gmineral under reducing conditions to form anhydrous
3 w M2 } q2 l' x) ltitanium tetrachloride, which is subsequently purified and converted to: |$ b6 d: {! C7 {
titanium dioxide either by direct thermal oxidation or by reaction with. }& j: G% g# s9 ^5 l, R
steam in the vapour phase. Alternatively, concentrated hydrochloric
* y5 O l# m% F) v, n! \3 \: L1 wacid can be reacted with the titanium-containing mineral to form a
3 L" Z# V ?9 u* X! Ksolution of titanium tetrachloride, which is then further purified and. S3 K6 i& D2 x. ?# h
converted to titanium dioxide by hydrolysis. The titanium dioxide is' o* X9 y/ j+ @- u, M3 b# z/ v& h
filtered, washed, and calcined.9 R2 [ K1 H; F
Commercial titanium dioxide may be coated with small amounts of/ L: h! ?& L# i& `5 t; H5 @
alumina and/or silica to improve the technological properties of the
$ M3 Q$ ?7 x' A0 x9 f* |+ bproduct.
% h# u) b2 M; X/ E" Y- d! Q( cC.A.S. number 13463-67-7
0 K- o4 B. f/ I* K4 RChemical formula TiO20 |, s5 z' F% M e2 |3 ]& @
Formula weight
2 R Q: b% G: a* R9 H3 a0 A" r79.88
$ w$ e" ?) @4 M0 UAssay
2 f8 x" m" } O1 k! n+ i/ eNot less than 99.0% on the dried basis (on an aluminium oxide and. T, n+ S9 p1 p. f/ ~" f0 b
silicon dioxide-free basis)7 i+ l* f6 w( y4 _3 O
DESCRIPTION, @& d) t5 E/ z0 a6 X# l2 k
White to slightly coloured powder, L* e% J0 i6 x% C, y
FUNCTIONAL USES
0 c/ g0 _8 n0 _; [9 lColour
0 E* H; d' j7 Z" d/ F+ ~: ZCHARACTERISTICS$ r7 o0 }' w/ k' k/ O
IDENTIFICATION- y; o0 H+ K; x6 \ I
Solubility (Vol. 4)
9 p. O- G6 G" n( N: zInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
0 h/ f: \ f* bsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
3 w& j) E8 u9 vsulfuric acid.
# K3 T4 |! K- aColour reaction/ ~, F0 m8 E" }) R0 I0 }" u- n
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
+ `2 p* d6 p. o' v5 H0 H2 k" @sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
7 D3 |0 a# G4 O: |8 V0 Ewater and filter. To 5 ml of this clear filtrate, add a few drops of
& w8 T/ R' i y+ M! Khydrogen peroxide; an orange-red colour appears immediately.
+ j, i6 G! p( `- M. q7 APURITY
3 O! ^6 x( C/ ~, O5 ^1 mLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)0 ^" |. U4 Z6 }' |( ]8 a
Loss on ignition (Vol. 4)' q+ x: S" p- i( k H0 ^: v; `
Not more than 1.0% (800o) on the dried basis
' U' L- U$ H0 I/ b9 {Aluminium oxide and/or- R0 t! ^: S& e; L) ?* I6 ~* P
silicon dioxide
8 c( @5 p- m6 J4 qNot more than 2%, either singly or combined2 O: h: f) I& i& C+ z6 {7 {' T' @
See descriptions under TESTS' g+ }1 {1 T. F+ o' Y
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
" K! h6 n! A4 {- z2 ialumina or silica.
# G ^3 c) P0 i* TSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and8 }+ x0 x% ~) y1 Y' L0 x' e' f
place on a steam bath for 30 min with occasional stirring. Filter
) }% y4 t$ R" cthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
4 c( f1 j4 k& s# i0 Lwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
1 u; d+ J9 r# [' n Fcombined filtrate and washings to dryness, and ignite at a dull red8 ?7 ?$ q4 r' I+ O) A
heat to constant weight.
+ g0 K2 Q! M! ^. ?6 RWater-soluble matter6 T" D" A r* [$ \2 v
(Vol. 4)
0 n @+ E9 v) e2 {( ?/ i CNot more than 0.5%$ w$ n* d7 d! k
Proceed as directed under acid-soluble substances (above), using
1 N- ?5 J( S9 t5 k2 @water in place of 0.5 N hydrochloric acid.9 L% j. L5 E) A. p3 h! |
Impurities soluble in 0.5 N
+ D" N: G; P; b6 H( r, L6 _5 n* t) ehydrochloric acid
8 W. Q- t# G. a0 |; n4 }Antimony Not more than 2 mg/kg. a$ ?5 G+ q9 E/ Q& @
See description under TESTS6 a' n; W' j3 A$ y: C0 H
Arsenic Not more than 1 mg/kg @/ I1 F. t! p
See description under TESTS9 D: ?: s s# V9 o9 U, f
Cadmium Not more than 1 mg/kg$ M' y9 T* v! K/ u
See description under TESTS
* d) i9 m$ E" pLead
7 T9 V8 y. p3 DNot more than 10 mg/kg; q7 |" r8 H/ f( N
See description under TESTS5 S% p2 R# y* K+ I, ^
Mercury (Vol. 4) Not more than 1 mg/kg
3 U& l) \: S! s" W( @1 IDetermine using the cold vapour atomic absorption technique. Select a
& S' O# ?( A9 L+ [6 }7 x( ysample size appropriate to the specified level
7 B/ k- J4 _2 D2 e7 y: @) J8 X) tTESTS: N$ w( }+ P7 \5 P6 P3 w
PURITY TESTS4 @# j4 z1 D, ^. }: @$ z
Impurities soluble in 0.5 N
8 w4 g$ ?0 t3 b. B; nhydrochloric acid
; {/ t- M$ I* q/ B9 OAntimony, arsenic,
: R/ r. }/ P% P1 n8 `2 \: Icadmium and lead
6 I7 v3 P( I( v+ N ~(Vol.4)/ Y! F' t# b! s# `0 h6 a# ?' C* e
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
9 s, A- ?( P7 @0 e; ]+ _5 ihydrochloric acid, cover with a watch glass, and heat to boiling on a* L8 R0 q# {+ \
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml; s, W$ }$ c) Y9 \+ R
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
; \4 C/ B+ ^' v* B6 o8 |$ ]/ B1 R4 Amaterial settles. Decant the supernatant extract through a Whatman
4 [) Y# g0 }0 pNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml/ t! g9 y' T: r; P- i9 Q
volumetric flask and retaining as much as possible of the undissolved
3 O x% F- e, X+ w- Bmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
$ j k6 T; a" s- {! b) w% t% tbeaker, washing off the watch glass with the water, and pour the
+ q; v+ Z1 m/ E4 ycontents into the centrifuge bottle. Form a slurry, using a glass stirring
: B; U+ T) R" \7 e: B, mrod, and centrifuge. Decant through the same filter paper, and collect
0 Z$ W$ u7 h- V5 H2 ]- @the washings in the volumetric flask containing the initial extract.; g. f# u1 ~/ v. g
Repeat the entire washing process two more times. Finally, wash the
8 @! O5 k6 a# `filter paper with 10 to 15 ml of hot water. Cool the contents of the flask' e! L8 w4 {. B5 J8 d& u, n! p
to room temperature, dilute to volume with water, and mix.
9 N! V9 O' ]% B! h9 Z S+ T/ IDetermine antimony, cadmium, and lead using an AAS/ICP-AES
& \) s: ~# `/ y i' j& Rtechnique appropriate to the specified level. Determine arsenic using the! m4 J& H$ G2 n2 I3 s4 P' ?( e
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
& w9 {. s+ _+ U' O- Q8 \3 @Method II of the Arsenic Limit Test, taking 3 g of the sample rather than& ]. }3 e' |! I( H5 x R
1 g. The selection of sample size and method of sample preparation
; b! _+ O9 j' I1 \) m& o( Vmay be based on the principles of the methods described in Volume 4.! j" h& z; u% N& }, S9 j
Aluminium oxide Reagents and sample solutions
3 }6 K& H' f$ i( k; ]- j0.01 N Zinc Sulfate: `+ N0 F+ g l
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to- a) v; g+ U, U3 _( ]
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg4 J" u5 a' ^! G( ]+ \& s# h
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
/ H8 u( @5 c# j0 f7 xconcentrated hydrochloric acid, heating gently to effect solution, then
" g* w2 s9 M3 o2 o8 ]transfer the solution into a 1000-ml volumetric flask, dilute to volume
3 q; I. ~& F6 a1 c3 {; A7 r6 Lwith water, and mix. Transfer a 10 ml aliquot of this solution into a 5009 E- G4 p1 ]* e( Z% z
ml Erlenmeyer flask containing 90 ml of water and 3 ml of6 @/ O w' c" E
concentrated hydrochloric acid, add 1 drop of methyl orange TS and0 J0 N8 B8 O k: u# C
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
. G0 c) V1 w: _4 {# d( e7 Edropwise, ammonia solution (1 in 5) until the colour is just completely
% J+ Z. g, e+ d- Lchanged from red to orange-yellow. Then, add:
) W8 {1 f% E5 Y1 |(a): 10 ml of ammonium acetate buffer solution (77 g of
4 v6 y9 D8 ^+ Uammonium acetate plus 10 ml of glacial acetic acid, dilute to
- ]( x8 [6 [5 L F/ q3 X" T1000 ml with water) and7 G: T w" k: | J( J% E
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
2 r% ?5 M# z7 k7 ]- X0 x$ Nof diammonium hydrogen phosphate in 700 ml of water,/ L& q" j. S! y- c# W# F7 n
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,5 F" e4 X" X, [4 p
then dilute to 1000 ml with water).
/ v+ ^9 i9 d+ Q' J2 O4 ]Boil the solution for 5 min, cool it quickly to room temperature in a2 h' [& N, d. x" d
stream of running water, add 3 drops of xylenol orange TS, and mix.
! X# U+ w) N8 B- p4 E3 dUsing the zinc sulfate solution as titrant, titrate the solution to the first& A1 N; k5 Q/ k* \/ q1 z; [) n
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:' X$ r/ B9 K3 v) S( D3 q3 V
This titration should be performed quickly near the end-point by
( b6 }9 S3 ~0 ~7 Y8 badding rapidly 0.2 ml increments of the titrant until the first colour
W X( T! a& s2 k' schange occurs; although the colour will fade in 5-10 sec, it is the true! ~% ?7 s* o% o4 y7 S7 Q
end-point. Failure to observe the first colour change will result in an* u7 a+ {' a% f6 c. E- T& b& \# z
incorrect titration. The fading end-point does not occur at the second$ ?7 ^2 q) g" W4 s
end-point.)
, C Z7 ~/ d6 U6 `) C0 i2 cAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
5 i. \3 |' z; X6 mstream of running water. Titrate this solution, using the zinc sulfate
& p" U5 w9 P$ [8 L8 c7 X" M; z( J& C! [/ Xsolution as titrant, to the same fugitive yellow-brown or pink end-point1 K- A( G. T( ]
as described above.
d0 ]' h0 e0 LCalculate the titre T of zinc sulfate solution by the formula:
, A- @$ p* L3 W4 OT = 18.896 W / V) ~6 Y. a* y- Q
where
* g. r. G+ Z |4 g8 KT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
: }5 r+ n% h1 d3 r7 RW is the mass (g) of aluminium wire3 r- R+ t* x# N2 J
V is the ml of the zinc sulfate solution consumed in the
/ _: j5 s( R4 ]+ g/ Dsecond titration
- w) A1 L' I j- ~: n% U3 z; C18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
- U- }& ^/ k: jR is the ratio of the formula weight of aluminium oxide to q2 ~* A" _4 H+ f* e
that of elemental aluminium.
0 W2 z8 S$ l U0 ^0 hSample Solution A" S5 Z+ Q$ Z. p _ Z5 S
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica1 V3 K3 A3 I4 G# V6 `0 e$ d
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).2 b% H* d& @& _* J+ d' U0 p
(Note: Do not use more sodium bisulfate than specified, as an excess% T+ b. p, N+ v+ Q: e6 @5 U% T4 k
concentration of salt will interfere with the EDTA titration later on in the; I% K$ F+ v9 U& C; ?6 E
procedure.) Begin heating the flask at low heat on a hot plate, and! _) p7 W' n8 ~
then gradually raise the temperature until full heat is reached.% w' U/ D. \1 y
(Caution: perform this procedure in a well ventilated area. ) When
0 k. C: U. S6 ?% C1 |5 a. r3 lspattering has stopped and light fumes of SO3 appear, heat in the full
5 `3 l7 k, f, U: W7 l- Rflame of a Meeker burner, with the flask tilted so that the fusion of the
* y, ?8 S$ a5 u% \9 v& Hsample and sodium bisulfate is concentrated at one end of the flask.
. S6 ~! Q' @9 z R( X8 C8 L3 cSwirl constantly until the melt is clear (except for silica content), but
4 |: b* c3 j' Kguard against prolonged heating to avoid precipitation of titanium! F+ w4 [1 m6 d; D6 F6 Q
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until& t, f; q- R5 j3 x" B# t
the mass has dissolved and a clear solution results. Cool, and dilute to+ W% M; |4 c& R8 r# G6 z& A
120 ml with water. Introduce a magnetic stir bar into the flask.
$ l: _! \+ h1 H8 Q8 RSample Solution B4 {4 A+ a# p* Q. H' s: D! ?6 N
Prepare 200 ml of an approximately 6.25 M solution of sodium
1 J" i6 ~! m$ w; n0 G' Shydroxide. Add 65 ml of this solution to Sample Solution A, while
J, r- b3 C/ D5 _/ J' ]! z rstirring with the magnetic stirrer; pour the remaining 135 ml of the9 l! i8 ^3 {; {
alkali solution into a 500-ml volumetric flask.( \ O+ Y7 v( s
Slowly, with constant stirring, add the sample mixture to the alkali
& |7 ~; ^. b: Psolution in the 500-ml volumetric flask; dilute to volume with water,% C2 M r' Z$ R7 p& A
and mix. (Note: If the procedure is delayed at this point for more than
9 @; S' Q; Y- ^4 a: m+ m5 t6 d2 hours, store the contents of the volumetric flask in a polyethylene
+ a1 \$ D2 c& m7 c1 p, Y' ibottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
' ?4 K2 P( h2 D. r" ` a1 Gthen filter the supernatant liquid through a very fine filter paper. Label
4 N$ g o( d8 A$ L# L" p- W8 ^: sthe filtrate Sample Solution B., e- G# r# ^9 ?" I# V! _
Sample Solution C
0 `0 Y8 C0 \9 Z; j# bTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer. G$ B2 `% U7 I2 X
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
# y f7 E& N4 H. G/ w( F+ \solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02; d; e. P1 f5 D( Y! ~
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is5 I. p- I8 V8 D" v5 O+ @
known, calculate the optimum volume of EDTA solution to be added, L+ q5 `6 V# D5 u7 E% p$ `4 [0 @
by the formula: (4 x % Al2O3) + 5.]# u4 t# E. p' B, S" L! n/ L7 X; F6 ]1 O
Add, dropwise, ammonia solution (1 in 5) until the colour is just
. M3 O/ Q$ u, Ucompletely changed from red to orange-yellow. Then add10 ml each( A* [9 R" [4 P2 R: F0 {) `
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to: c4 |$ m/ M1 B. s; D
room temperature in a stream of running water, add 3 drops of xylenol
* |7 l2 G8 o% {' {9 X$ d" K: oorange TS, and mix. If the solution is purple, yellow-brown, or pink,
! n2 V4 D/ m8 Z N0 x- L- ybring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired2 E* ?" z+ K9 o& d
pH, a pink colour indicates that not enough of the EDTA solution has
3 f& P& h0 L8 m! p2 w, _; P1 Nbeen added, in which case, discard the solution and repeat this Y: [3 p0 k* E6 J/ {
procedure with another 100 ml of Sample Solution B, using 50 ml,
" Y# G/ G4 r) f0 u/ zrather than 25 ml, of 0.02 M disodium EDTA.$ L4 D. l3 `5 C! w$ A
Procedure
6 Q1 V1 Y4 N4 fUsing the standardized zinc sulfate solution as titrant, titrate Sample3 `5 i8 M3 z! u& [$ X4 \1 }+ i
Solution C to the first yellow-brown or pink end-point that persists for
" L! A$ s7 ?- k3 u# Y8 r5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first+ j4 |# G4 d/ ^- h1 {
titration should require more than 8 ml of titrant, but for more accurate
; i9 O Q0 K5 f" |* ` gwork a titration of 10-15 ml is desirable.
9 @0 \4 w& ` G3 f$ |Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
2 N. |6 v( R _* v5 Xmin, and cool in a stream of running water. Titrate this solution, using) A7 M5 v2 T' M
the standardized zinc sulfate solution as titrant, to the same fugitive% g( }* e7 z$ F( M: U
yellow-brown or pink end-point as described above.6 o4 H7 ?3 K _4 }- L
Calculation:
/ m& x, Z, i9 g' B9 |$ w6 K; lCalculate the percentage of aluminium oxide (Al2O3) in the sample
( {5 O: X% b2 z1 n8 C2 O- M; _taken by the formula:9 N; n1 g5 ]* Y: h2 s
% Al2O3 = 100 × (0.005VT)/S! H, J) G& e* d/ [4 v. d1 A3 o
where
: H8 D/ V6 }* ^8 UV is the number of ml of 0.01 N zinc sulfate consumed in r) m$ A; [! J4 u
the second titration,
; d9 w! {) @1 E0 L: x9 QT is the titre of the zinc sulfate solution,; _& T. l, X0 ~, S J8 j
S is the mass (g) of the sample taken, and
f9 n1 Z# v/ |0.005 = 500 ml / (1000mg/g × 100 ml).
" @- D$ v2 q& ?Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica9 z# \7 f# F" i$ m; z( |
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
+ m! F7 i* x u/ V( ?# X: dHeat gently over a Meeker burner, while swirling the flask, until' [ H. W' p$ m; J! q. \: f
decomposition and fusion are complete and the melt is clear, except
; I! v; U7 I6 `6 Z* n/ Y9 nfor the silica content, and then cool. (Caution: Do not overheat the
! }: E* U+ L R6 F2 K# ucontents of the flask at the beginning, and heat cautiously during
6 C9 s; T" @& [" Gfusion to avoid spattering.)
@) t# ]* ]9 aTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
% r7 T4 _ G6 J( z, Vcarefully and slowly until the melt is dissolved. Cool, and carefully add- M4 [( m( f, w! b" U
150 ml of water by pouring very small portions down the sides of the% \. M0 v L% ] i7 y4 J% R
flask, with frequent swirling to avoid over-heating and spattering. Allow4 v+ P$ E- K: e4 z; q. ^
the contents of the flask to cool, and filter through fine ashless filter, B- U% _2 a% W9 I7 N" Z
paper, using a 60 degree gravity funnel. Rinse out all the silica from% `/ w- g k0 |& _5 z! V' x9 _1 s
the flask onto the filter paper with sulfuric acid solution (1 in 10).! S J3 U0 F: M0 o
Transfer the filter paper and its contents into a platinum crucible, dry in
; a9 a; w6 H$ Ian oven at 1200, and heat the partly covered crucible over a Bunsen
8 ~2 ~* w, }5 v% }+ i9 r* ~burner. To prevent flaming of the filter paper, first heat the cover from
v3 Y/ M' C1 P; p! h3 v7 t6 b! dabove, and then the crucible from below.
0 W( [, j' F& k7 k" [8 w( v- uWhen the filter paper is consumed, transfer the crucible to a muffle
1 T; f$ y% S# J3 n+ Q bfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and( e. X. @( b9 ?; c
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
- v7 E& b7 j+ @- thydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
3 `: S7 k: }5 H( @on a low-heat hot plate (to remove the HF) and then over a Bunsen# N% ?# E6 _. b4 D- l. T$ I
burner (to remove the H2SO4). Take precautions to avoid spattering,0 @0 l. U6 o& G( ]
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a% F+ j6 T7 [5 s7 u3 E: ]% J
desiccator, and weigh again. Record the difference between the two% L; P6 G }8 C1 _2 _- N: A" {
weights as the content of SiO2 in the sample.
! g4 v" t' v- O( Q+ g- {, dMETHOD OF ASSAY* x% {6 U. X4 L; y
Accurately weigh about 150 mg of the sample, previously dried at 105o6 P* a7 {) s. r3 S _6 m1 Y
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
8 L+ @& A# x. O! d- G) Z/ T. fand shake until a homogeneous, milky suspension is obtained. Add 30
% o, o7 p0 ?4 W# hml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
" |5 m1 d" u* _9 G3 b9 t3 S0 O) M# theat gently, then heat strongly until a clear solution is obtained. Cool,
S M* }% I( m1 n6 P- {then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
9 n2 `/ T$ B/ ?/ }5 n& Jacid, and stir. Add 3 g of aluminium metal, and immediately insert a
* k1 ?8 v' L( ~& l* {* K7 Prubber stopper fitted with a U-shaped glass tube while immersing the
6 K1 O3 x! n/ U2 Dother end of the U-tube into a saturated solution of sodium. x" v3 r' ^8 m) O6 Q* b8 m- s
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
" z1 P3 z5 r, E0 `) c* Ahydrogen. Allow to stand for a few minutes after the aluminium metal) |+ F% K0 S+ W6 {" A# {
has dissolved completely to produce a transparent purple solution.2 e: [ S! M" q$ ]2 D& A5 u5 ?
Cool to below 50o in running water, and remove the rubber stopper
" C% Z' r0 G/ `% h9 A' ecarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
+ p4 Y0 a6 E& Gsolution as an indicator, and immediately titrate with 0.2 N ferric
9 Q! q5 q0 \& ?& D, Iammonium sulfate until a faint brown colour that persists for 30
0 d4 m# M, ?/ J2 m/ xseconds is obtained. Perform a blank determination and make any" L$ C% F" U- E4 e" q4 `. m
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
! L) _3 M3 _4 y& a# D2 Uequivalent to 7.990 mg of TiO2.6 e+ u) k ~& t. G
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