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二氧化钛(钛白粉)
二氧化钛(钛白粉): m% s% L/ I3 v: T6 `8 y
) f7 F: N( Q5 n) K1 ?JECFA关于二氧化钛(钛白粉)的结论
1 \7 @" \- Y3 `( [; F* a
3 o* o. W, j- W摘要: 2006年JECFA关于二氧化钛的结论
+ F0 b: E+ H$ E y7 U& ^/ P7 J0 lADI值:不作限制。3 w; t+ V: O3 w3 [3 O
功能:着色剂9 I* B: {: u5 z; i' U3 ^: C* E
/ c/ |8 D2 a. [5 `4 y- K6 j3 }TITANIUM DIOXIDE
! w V# e3 v1 A& s6 QPrepared at the 67th JECFA (2006) and published in FAO JECFA; _9 X1 x1 f0 q9 G/ B6 @
Monographs 3 (2006), superseding specifications prepared at the 63rd
?4 t9 A9 V7 Y! }. q. L9 R, U4 w& XJECFA (2004) and published in FNP 52 Add 12 (2004) and in the. @& d* d9 J. l" M. [5 z# `. Q! f7 a
Combined Compendium of Food Additive Specifications, FAO JECFA
# E s! S; r! Q4 uMonographs 1 (2005). An ADI “not limited” was established at the 13th7 U+ e0 y; Q0 f) t
JECFA (1969).
% T. y/ \ }2 z/ L8 x2 g; _SYNONYMS" [7 }3 i# x4 ?% v! u" U' `
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171, H) d' w# T' m1 C" k' R$ p# ]+ _
DEFINITION |9 e7 o1 \& y
Titanium dioxide is produced by either the sulfate or the chloride% G$ s9 F/ T" Q$ d0 z' Y
process. Processing conditions determine the form (anatase or rutile
* b+ r1 h ]- a+ Zstructure) of the final product.' }& n g2 H8 d* j8 c8 d0 V
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
1 S4 q5 P8 c `or ilmenite and titanium slag. After a series of purification steps, the
0 A& R: m" ?+ M: Q8 ?7 ^isolated titanium dioxide is finally washed with water, calcined, and/ V# b2 @ S) N# m! [4 m
micronized.
/ _, ]( ?- u7 P1 q2 _In the chloride process, chlorine gas is reacted with a titaniumcontaining
% \$ U# z; `+ W5 u. q1 u) t4 Lmineral under reducing conditions to form anhydrous
6 E7 W" _- |9 ?' S- Wtitanium tetrachloride, which is subsequently purified and converted to; L: @! f" a4 R/ a4 ?; o
titanium dioxide either by direct thermal oxidation or by reaction with0 H5 }! i$ v% S. y$ F) B
steam in the vapour phase. Alternatively, concentrated hydrochloric/ _( P1 S; T, Y- G; x
acid can be reacted with the titanium-containing mineral to form a
, m" j2 A' j7 l- E0 {- ?solution of titanium tetrachloride, which is then further purified and( E3 D1 \% c+ p1 m* ~) R, F9 v
converted to titanium dioxide by hydrolysis. The titanium dioxide is9 {! ]4 ^+ ~/ p
filtered, washed, and calcined.2 W! S$ a- n: [* ^2 R! s: a
Commercial titanium dioxide may be coated with small amounts of, _9 V& m6 C) |2 m0 f
alumina and/or silica to improve the technological properties of the( U4 M; @3 r5 s* N+ u
product.7 ?! ^2 L( j! Z5 o6 ^
C.A.S. number 13463-67-7
1 z5 z5 W" ]& l. c5 E0 h% {7 FChemical formula TiO2
" ~2 q' p6 ^% P; l, J0 s# W1 sFormula weight
. N5 ~) r9 r8 l* B0 O" ?3 y79.88, J) P F B3 C
Assay
% Y) ?9 J4 u/ p# ?Not less than 99.0% on the dried basis (on an aluminium oxide and+ X$ Y3 y4 T' }+ L% ?5 V* m
silicon dioxide-free basis)
* C! g5 P( f: a5 jDESCRIPTION
! ]- f4 K; p6 ~1 LWhite to slightly coloured powder# q- @ W9 F7 f3 i, D
FUNCTIONAL USES
( a8 ^& E% ?7 P$ |0 V, YColour
- w3 Q3 @! z' V7 R+ _CHARACTERISTICS5 A& ?/ j. q- G5 A
IDENTIFICATION
0 ]1 H* L/ Q o! |1 DSolubility (Vol. 4): _7 v2 y$ U7 Y& r+ | ?
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
, D+ q( C9 \, W* y; csolvents. Dissolves slowly in hydrofluoric acid and hot concentrated: L* U/ Z5 U) Q
sulfuric acid.
2 o; R* z. _2 _; }* K/ [* GColour reaction
) c; O( Z6 A9 b4 o, D) KAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
' |$ Y A7 i( l3 x8 lsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
' p- H$ n+ u% C4 w+ Lwater and filter. To 5 ml of this clear filtrate, add a few drops of
' S |9 x, I4 h& } Mhydrogen peroxide; an orange-red colour appears immediately.& n/ Z( r5 ]1 A: j$ L. J' g5 S
PURITY
; S9 }, a, l9 ?* v# q. LLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)9 r' a a3 z/ E; e2 v9 X+ B# a
Loss on ignition (Vol. 4)
r4 k- d* B8 I n9 x7 I. cNot more than 1.0% (800o) on the dried basis
; I q) y$ E2 h0 ^- D- {" YAluminium oxide and/or
( s6 O, ~# e# I6 w7 A/ k; M8 Osilicon dioxide
# u6 d9 H' o/ h) k3 lNot more than 2%, either singly or combined
4 a$ d1 |* \4 Z4 h+ o, i! LSee descriptions under TESTS+ g6 w7 M4 W* r' L, S- z' e/ N' k
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing: P+ n8 l3 F/ [- j: l& }
alumina or silica.4 X g( h/ i& U: e
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
8 h. L8 I/ o& x' S+ d& a% z+ pplace on a steam bath for 30 min with occasional stirring. Filter
1 e) E: o! s; F, Xthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
1 [: M, `% ^+ R8 n1 ^' b% u. \with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
. q, K6 r8 V8 H. j& r6 Gcombined filtrate and washings to dryness, and ignite at a dull red
3 T2 r* A% C" O+ N. c; {( Y+ dheat to constant weight.4 ^; }! A( m5 g- H
Water-soluble matter( [+ I1 }/ J7 s0 @
(Vol. 4), V1 y) x; z+ @/ j
Not more than 0.5%
) j8 M1 g \& i7 yProceed as directed under acid-soluble substances (above), using
" {+ c; C6 V _' I% ]9 o) V6 i2 ?1 G( ewater in place of 0.5 N hydrochloric acid.
. x5 w3 F6 [+ M+ ?5 AImpurities soluble in 0.5 N
4 m( `$ \# H5 t' k8 x$ R. }hydrochloric acid" R7 p; `7 u$ I4 I8 E
Antimony Not more than 2 mg/kg
9 @* j. X5 q& E+ \See description under TESTS& s' R2 L( P+ B/ X& I; b3 ?$ U
Arsenic Not more than 1 mg/kg
+ E3 S# C- W8 A& LSee description under TESTS
- C+ J: X! q1 Q0 U; J. g/ U3 SCadmium Not more than 1 mg/kg
/ s* X! C, d) m/ x8 _See description under TESTS
5 B: y- o6 Q' Y4 ^% ?# yLead
, h1 C5 R# I7 r& [- dNot more than 10 mg/kg+ T/ k1 c% k' X" Y
See description under TESTS
% n% _- B& M u+ x* H1 }Mercury (Vol. 4) Not more than 1 mg/kg
, H2 x* D' f% |3 {. f0 m$ ODetermine using the cold vapour atomic absorption technique. Select a
3 P# x' Q1 b0 ?. M! L! q7 Y' R Y9 ?, xsample size appropriate to the specified level* I- @+ y R1 J+ d" d
TESTS5 b: o0 c8 r0 {+ Q" ]
PURITY TESTS
9 D/ B; P1 y1 b% k1 k- y! nImpurities soluble in 0.5 N
! v: a; I/ ]6 v9 ?! r8 k3 Ghydrochloric acid9 o+ r8 J& e* K( Z( t/ |" y
Antimony, arsenic,
4 d, c2 b- D" Icadmium and lead" r, k0 F' z/ `: m: c3 W. E% y
(Vol.4)
$ E$ {: f/ Y* w( z! C! i6 `6 ?& |" `Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N* r: X0 I) X4 F7 F& u7 @
hydrochloric acid, cover with a watch glass, and heat to boiling on a0 ?% z: a, U8 `" `$ b+ l6 h- K
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
* r0 g$ X* X B2 Q& icentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
- l( o8 F- C- Z$ i* v6 Vmaterial settles. Decant the supernatant extract through a Whatman
* t+ Z8 `7 r" e$ @No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
" z, Y; }; [0 D1 fvolumetric flask and retaining as much as possible of the undissolved
$ Z0 @- _+ O3 g& |6 ]# l7 Jmaterial in the centrifuge bottle. Add 10 ml of hot water to the original6 K( b" |4 I1 P3 c& P
beaker, washing off the watch glass with the water, and pour the1 Y( c" D* D+ t4 ?6 G( \3 H
contents into the centrifuge bottle. Form a slurry, using a glass stirring6 O9 Q; [ P* Z9 ^0 l7 u
rod, and centrifuge. Decant through the same filter paper, and collect$ X {3 p% c: b5 D
the washings in the volumetric flask containing the initial extract.
- H+ D( Q9 M/ ]9 ]Repeat the entire washing process two more times. Finally, wash the( w) v' \5 J( I# w- c# u
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
/ Y$ v3 j( L7 @& pto room temperature, dilute to volume with water, and mix.
9 Q6 U! L( `+ v. U' T/ W8 C0 PDetermine antimony, cadmium, and lead using an AAS/ICP-AES
* S' U0 Z3 Z3 Q! ]: Ttechnique appropriate to the specified level. Determine arsenic using the- B3 r$ g. ?, Q3 X' m7 e
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
: B3 g4 D5 n& \% w2 G. q( XMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than1 ^( b. H8 ~& V3 q. N& z& |
1 g. The selection of sample size and method of sample preparation
( i6 C. s5 t! Amay be based on the principles of the methods described in Volume 4.9 Z2 |9 Z5 n X$ W: m6 \
Aluminium oxide Reagents and sample solutions
$ ?4 {8 J* k" [) D, Y0.01 N Zinc Sulfate
7 D. Z( `2 d8 J8 \4 a. vDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
8 T( |# W. C9 N6 O; R& _- j1 |make 1000 ml. Standardize the solution as follows: Dissolve 500 mg8 ?3 O! J) O7 f: F
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of$ e9 S3 U2 z' P1 e
concentrated hydrochloric acid, heating gently to effect solution, then
" u/ G1 y! t+ v/ etransfer the solution into a 1000-ml volumetric flask, dilute to volume
; Y" W! g4 A& Y& [/ s K5 g1 mwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
# o# s. s9 i5 Z# ^1 ]" _; L0 Jml Erlenmeyer flask containing 90 ml of water and 3 ml of9 f) P ~6 f; D7 q% @
concentrated hydrochloric acid, add 1 drop of methyl orange TS and2 o: A& m1 L! C b" K1 a
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
/ p, v7 c5 f" h) g& z$ A% S/ Hdropwise, ammonia solution (1 in 5) until the colour is just completely
{" G% N; q- b7 S( k) v w. echanged from red to orange-yellow. Then, add:
, [! t3 F7 i% C8 [4 [' h; i(a): 10 ml of ammonium acetate buffer solution (77 g of9 F4 z0 C1 B: D8 s! h. R+ `
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
$ n7 }( N# e* X: z/ d$ L" k) ?* |1000 ml with water) and
4 K( V% R6 T1 ?6 y, r- D(b): 10 ml of diammonium hydrogen phosphate solution (150 g; I0 u" v/ U, D
of diammonium hydrogen phosphate in 700 ml of water,
2 B+ u$ N1 b1 V$ X1 }9 g; ?6 S" i H4 badjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,, g8 ?* D4 B, l7 J4 S+ [
then dilute to 1000 ml with water).# M8 z; ]( @/ P+ p
Boil the solution for 5 min, cool it quickly to room temperature in a4 x7 l2 p7 ^1 J' |
stream of running water, add 3 drops of xylenol orange TS, and mix.
6 g) W: C9 R. m( T; RUsing the zinc sulfate solution as titrant, titrate the solution to the first+ ^7 B5 o: C: x" n# s" r/ k
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
* P2 [' V1 H$ Y, x6 M9 Z, mThis titration should be performed quickly near the end-point by- y' m4 {7 q0 B$ z3 l# D( |) D6 p
adding rapidly 0.2 ml increments of the titrant until the first colour6 _3 Z& q" v) I1 b" m
change occurs; although the colour will fade in 5-10 sec, it is the true
0 ?3 W/ ^# q- l" U3 _. O- V) }end-point. Failure to observe the first colour change will result in an
, g4 ]+ l. f" S' v+ \8 H5 [incorrect titration. The fading end-point does not occur at the second
% C/ A. k+ ?9 e/ ^3 {% [end-point.)
. M* G0 y: T3 V' xAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a1 [/ I, l; p: Z: }, Z
stream of running water. Titrate this solution, using the zinc sulfate
" s% a8 X! R+ y; s2 L M7 a( ^solution as titrant, to the same fugitive yellow-brown or pink end-point
: a/ x. b9 n" L6 tas described above.
" j; `! h' e! ICalculate the titre T of zinc sulfate solution by the formula:
5 O9 a/ F8 q& j+ U5 U) k, tT = 18.896 W / V2 R: ~8 B# v& x
where
" D0 Z3 B( [1 i+ p1 q8 z0 r% NT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
$ H$ B4 {* |; S# qW is the mass (g) of aluminium wire3 U. k! m5 N- v5 W ?* J( ~8 d: A
V is the ml of the zinc sulfate solution consumed in the4 q1 t/ ~0 _+ j( |
second titration
' n; |$ E% ~9 H* {, B, ?. v18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and: |3 ^( _7 O" g& a" C+ a
R is the ratio of the formula weight of aluminium oxide to8 K1 \/ a: R5 h; d
that of elemental aluminium.
) Q6 D3 s, `& v5 @* l ~/ @Sample Solution A7 F' U, Y3 H/ R
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
7 t; `, U- b* `" ^% x* v$ Pglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).! e1 v1 s l) S9 z$ n7 F/ ^$ _. B
(Note: Do not use more sodium bisulfate than specified, as an excess
8 u# ]* ~1 H( u' c$ q; Q! B" h% ~concentration of salt will interfere with the EDTA titration later on in the
: |$ Z9 D( M9 A' m# C) q; _" r5 g' Oprocedure.) Begin heating the flask at low heat on a hot plate, and
) s% n# V$ y2 u" ^4 C9 |then gradually raise the temperature until full heat is reached.
% q! f: ] {% {$ D(Caution: perform this procedure in a well ventilated area. ) When
% N% a) H r- I+ zspattering has stopped and light fumes of SO3 appear, heat in the full- ^- P _& k9 p; P `" K9 S! o* [
flame of a Meeker burner, with the flask tilted so that the fusion of the9 L' ?3 r8 ]' a( E- u3 y2 W
sample and sodium bisulfate is concentrated at one end of the flask.( `3 E6 O4 `2 `* f- R* u
Swirl constantly until the melt is clear (except for silica content), but8 q" I& F7 W6 ?0 b4 {! ] N0 X
guard against prolonged heating to avoid precipitation of titanium
! K, B6 ?/ f+ a v; s3 ]dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until! {$ d- r- W f1 W: }0 Z
the mass has dissolved and a clear solution results. Cool, and dilute to
& Z& p' Z% k& Y* x3 R120 ml with water. Introduce a magnetic stir bar into the flask.
) I$ S9 N( j4 D2 y; L6 lSample Solution B( P3 k# z) _- ]) r: S; A& E
Prepare 200 ml of an approximately 6.25 M solution of sodium
' U- l! f, h3 _ R; ghydroxide. Add 65 ml of this solution to Sample Solution A, while
, ^$ x9 Q2 c6 i6 v" ^. A; n/ @stirring with the magnetic stirrer; pour the remaining 135 ml of the7 J8 _0 H- m+ I
alkali solution into a 500-ml volumetric flask.
( V8 {. `% Z; G) H# Z& b0 OSlowly, with constant stirring, add the sample mixture to the alkali, S- P! F f% [
solution in the 500-ml volumetric flask; dilute to volume with water,
h0 O% C8 x! D; |. E7 A' Gand mix. (Note: If the procedure is delayed at this point for more than! x3 E0 Q1 v$ y
2 hours, store the contents of the volumetric flask in a polyethylene% K1 W% V1 Y7 _/ B# N3 ^0 y( R
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),4 `' M3 L9 T+ s+ P) C; j8 Z
then filter the supernatant liquid through a very fine filter paper. Label
' ^. n8 t& D. q+ Sthe filtrate Sample Solution B.! c: }" A S; P* }
Sample Solution C% s2 F8 f9 W6 A3 O( q/ r
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
l$ e# r' R# V* Z. \0 i! ?. Fflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
& @1 H$ a& c* wsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02( M; D4 x+ H$ v. |5 V8 A+ d3 b
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is3 T/ B/ H1 M# P' A
known, calculate the optimum volume of EDTA solution to be added: [ P! W0 B6 S+ U/ t6 o% [' D% |
by the formula: (4 x % Al2O3) + 5.]
$ h2 Z2 ~# Q# g" GAdd, dropwise, ammonia solution (1 in 5) until the colour is just
, y% v( ^( }% ncompletely changed from red to orange-yellow. Then add10 ml each
% E4 F& e; I' t% u3 R% h/ z nof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
}2 ]5 y. j( N# z( E) n# lroom temperature in a stream of running water, add 3 drops of xylenol+ h3 C( l9 ? ~ Z- a
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
+ P, A: j. ?! \5 r; h# Obring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired: ?% A: T) O+ P
pH, a pink colour indicates that not enough of the EDTA solution has3 |8 R; l+ } }, m, l& E
been added, in which case, discard the solution and repeat this
4 g* X4 O- T: O- s G- Tprocedure with another 100 ml of Sample Solution B, using 50 ml, _" h& E- q% A6 k5 u- F
rather than 25 ml, of 0.02 M disodium EDTA.
( E/ Y& u+ \+ t+ \, [Procedure
) p& N m# J% `; v# X2 aUsing the standardized zinc sulfate solution as titrant, titrate Sample/ ^$ R& y4 `2 z- R
Solution C to the first yellow-brown or pink end-point that persists for3 ]( ~( t0 U* }7 a' Z, ] s
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first" u& ^, y6 M7 Y$ C7 u4 p5 V0 F' H
titration should require more than 8 ml of titrant, but for more accurate5 u- O$ }) J- Z' ?/ k
work a titration of 10-15 ml is desirable.
- h8 w1 E3 `0 A- ]8 _Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
- t/ M4 q. O0 b% D4 zmin, and cool in a stream of running water. Titrate this solution, using# H1 Z' r/ C* A# M' S* `
the standardized zinc sulfate solution as titrant, to the same fugitive
4 W* G* b- G: i: S. y, Lyellow-brown or pink end-point as described above.
( ]: F& h3 {& P) \Calculation:
) O( @7 a6 ]$ K }Calculate the percentage of aluminium oxide (Al2O3) in the sample
' d0 q$ z7 j' E- Vtaken by the formula:
4 P7 j( v* U, c% Al2O3 = 100 × (0.005VT)/S
( z2 K1 v9 C$ l5 p! h3 kwhere! J6 W. }, s3 F9 V1 {
V is the number of ml of 0.01 N zinc sulfate consumed in0 F# }( f v3 K9 p
the second titration,; `" g! o, n r& z
T is the titre of the zinc sulfate solution,1 b* J2 [# O7 V; D
S is the mass (g) of the sample taken, and
7 K. z9 f) ~& I1 i9 T! i; _0.005 = 500 ml / (1000mg/g × 100 ml).) L3 i0 R/ |' x% S: |0 ]& S9 u! D7 n
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
6 a- Y# m9 p+ I0 j6 I- ]- Y" @- _glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O)./ ]) x% ?' `$ H' E: Y
Heat gently over a Meeker burner, while swirling the flask, until/ [9 Z) T6 `! q9 a+ T$ k. I
decomposition and fusion are complete and the melt is clear, except; ^8 i0 }8 |' j9 d, e
for the silica content, and then cool. (Caution: Do not overheat the' H0 w% {9 u: v, Z
contents of the flask at the beginning, and heat cautiously during3 |% G4 v! L! E: s
fusion to avoid spattering.); T+ }2 N" S9 c: v. i3 S. E; p
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
. k3 I: I( u- K# l5 R& ccarefully and slowly until the melt is dissolved. Cool, and carefully add" F/ S0 V+ L+ @% P
150 ml of water by pouring very small portions down the sides of the
: v6 Y. k4 v8 s# v) P# T. vflask, with frequent swirling to avoid over-heating and spattering. Allow
( i# b3 Q- N* @4 S% w2 ^ Uthe contents of the flask to cool, and filter through fine ashless filter. [+ t+ `9 _8 [1 @8 D
paper, using a 60 degree gravity funnel. Rinse out all the silica from
~- s, D1 \, H$ P# b9 A/ Xthe flask onto the filter paper with sulfuric acid solution (1 in 10).0 ^! L# V* @; t1 A3 \1 ]9 \. j
Transfer the filter paper and its contents into a platinum crucible, dry in
+ r' y4 X- i, I& tan oven at 1200, and heat the partly covered crucible over a Bunsen
+ ~5 o# G( I( j2 O: [: ]burner. To prevent flaming of the filter paper, first heat the cover from
# b! I- V) c ^/ habove, and then the crucible from below.7 U- C: e# b7 ]+ u
When the filter paper is consumed, transfer the crucible to a muffle
5 O' `9 Y- x" G& qfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and, {) ?$ |$ \ _* i
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
' ~& R# P8 x4 M- a: Khydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
+ V$ j7 Y9 x7 d0 ?! z, t( _6 non a low-heat hot plate (to remove the HF) and then over a Bunsen
' M2 h6 z; o$ fburner (to remove the H2SO4). Take precautions to avoid spattering,
) `+ k( C; C8 C4 _6 cespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a, \5 @* M0 O4 n5 ]1 A! m: `7 ^
desiccator, and weigh again. Record the difference between the two" ^7 }. I7 l4 b- A; b
weights as the content of SiO2 in the sample.( z5 z6 r; w8 h3 f
METHOD OF ASSAY% h: Y( V5 o3 o E( _! J- g) z
Accurately weigh about 150 mg of the sample, previously dried at 105o
% T0 e* ]- v! a7 Y# ?0 j5 dfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water0 ~1 P9 h' X. O) v6 G
and shake until a homogeneous, milky suspension is obtained. Add 30
/ q' ?/ \/ f8 N7 p0 b& s5 T# Vml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially& s* i9 T5 w3 n* z) }, q3 c. v
heat gently, then heat strongly until a clear solution is obtained. Cool," c- G8 m1 H6 p0 J. ^
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
8 [) e. k" n/ `6 eacid, and stir. Add 3 g of aluminium metal, and immediately insert a5 ~$ n% a% o& C* u
rubber stopper fitted with a U-shaped glass tube while immersing the0 A4 n, w( d( f
other end of the U-tube into a saturated solution of sodium' I& u5 _! J7 ` j0 a! V
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
5 s7 {* N4 [ z5 n, O& e% vhydrogen. Allow to stand for a few minutes after the aluminium metal
6 M& i+ R0 j; U( r7 q shas dissolved completely to produce a transparent purple solution.; P% D, W& `) ~, e$ z- N
Cool to below 50o in running water, and remove the rubber stopper
' P; T3 ?! V/ R4 H, `+ acarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate3 j3 p; n7 D5 ?& p9 a1 ?
solution as an indicator, and immediately titrate with 0.2 N ferric7 h% }1 j4 z( c. f5 Q
ammonium sulfate until a faint brown colour that persists for 30, X& Y$ L' A2 s2 z
seconds is obtained. Perform a blank determination and make any( {+ S2 v$ P# E
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
2 m2 @0 w) U2 n5 o2 n( w; `& y! p2 lequivalent to 7.990 mg of TiO2.4 H: [9 ? Y. R+ a% t- Z0 |
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