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二氧化钛(钛白粉)
二氧化钛(钛白粉)
V7 \8 P' M8 T$ [2 C( u
! H i6 X' d, m& A Q/ E7 G( J t% j# FJECFA关于二氧化钛(钛白粉)的结论; s2 I, ?1 z- d) L E; |
1 |8 I' p, h. V1 m3 i摘要: 2006年JECFA关于二氧化钛的结论6 o- y7 f7 M" B5 Z$ n' P; A) I
ADI值:不作限制。9 q! J4 K; f% R; s* G
功能:着色剂
& w6 {* R! }3 v1 p5 w* \8 W; Y& J/ c
TITANIUM DIOXIDE
. x1 w2 _1 A$ J# W9 I7 tPrepared at the 67th JECFA (2006) and published in FAO JECFA
- z" g8 ]3 `% e5 MMonographs 3 (2006), superseding specifications prepared at the 63rd
7 `, \; o0 g2 L8 ]( NJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
7 G; e/ m. H2 Y: O- t5 dCombined Compendium of Food Additive Specifications, FAO JECFA
2 b; _0 N" n; W# s; D) NMonographs 1 (2005). An ADI “not limited” was established at the 13th- v7 ~7 k& s1 N1 y, u1 b
JECFA (1969).
C" n; O3 F0 s. D8 h3 XSYNONYMS5 |; J" o+ c' R- T* Q
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
* r3 |- N4 z. C/ V; V+ WDEFINITION. U- |4 ?9 a2 O+ S, z5 G
Titanium dioxide is produced by either the sulfate or the chloride
. F# h* _5 |- A( V+ |9 ~% d: oprocess. Processing conditions determine the form (anatase or rutile
7 _! b3 X$ o( c0 Ustructure) of the final product.
& y; \, |8 ~6 S6 r, @1 S% XIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
5 q2 q+ u3 M" kor ilmenite and titanium slag. After a series of purification steps, the8 O4 U5 E2 n$ k$ I
isolated titanium dioxide is finally washed with water, calcined, and+ A8 ~4 S+ U* @: X" s
micronized.4 o# O# T( |& A3 N* \
In the chloride process, chlorine gas is reacted with a titaniumcontaining
* I5 E) a; _/ `5 Y& ^6 q) G- Gmineral under reducing conditions to form anhydrous" g! l5 Z( o. V. ^
titanium tetrachloride, which is subsequently purified and converted to; C8 ?% ~1 Y1 ~* D! Q* w, O' A1 I
titanium dioxide either by direct thermal oxidation or by reaction with
( }! j# Z( J( v4 y( @steam in the vapour phase. Alternatively, concentrated hydrochloric
+ l: K) m" g7 T. O+ macid can be reacted with the titanium-containing mineral to form a
: v6 F/ X2 O7 K Q7 qsolution of titanium tetrachloride, which is then further purified and
& J; p8 o9 B0 {* N4 D7 R3 i3 L7 Qconverted to titanium dioxide by hydrolysis. The titanium dioxide is
, W5 x$ p5 Q2 g% t& r+ R) Ofiltered, washed, and calcined.
0 V7 Z+ K6 `+ q8 m; \Commercial titanium dioxide may be coated with small amounts of
) p0 W, ~7 c9 M- |/ Ualumina and/or silica to improve the technological properties of the1 ]5 X7 V+ o o# W+ _# T( l7 D
product.) u- V8 v: V9 g+ z. V" \
C.A.S. number 13463-67-7) q k2 Q. i/ b4 \$ ?& J
Chemical formula TiO2- g4 n# ?3 I% C# k
Formula weight+ W- K5 o) T" O! v5 G0 S
79.88
6 A7 k6 t5 i+ N* n) H7 T" j8 V: LAssay
; J* @7 C6 c3 DNot less than 99.0% on the dried basis (on an aluminium oxide and
5 p/ T- v" C! F6 ]4 |$ ^- C3 Tsilicon dioxide-free basis)( p2 {8 Z6 v0 w- Q, `
DESCRIPTION& ?6 ^: h2 J+ H5 w
White to slightly coloured powder
* R' \$ l& j4 N, E" B9 YFUNCTIONAL USES
. O6 X) O) k, Q% K0 E- WColour
6 p, K" z/ k9 y. Y% A3 \4 D6 dCHARACTERISTICS
, | o8 w) p% P) b, TIDENTIFICATION
/ }$ p3 n# g) Q6 t4 gSolubility (Vol. 4)
2 F% m& { Y% }7 }# [' R/ F# W$ ZInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
0 ?/ Z# V0 c# V: Y3 p) J. G+ |! B) {solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
" e4 l' @: M) ssulfuric acid.$ Z: x8 ^0 y+ b, q
Colour reaction8 }5 ~# C8 s8 I7 W E. M
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
5 \0 E. a% n+ isulfuric acid appear, then cool. Cautiously dilute to about 100 ml with5 _4 b- J& \, U/ W# }; h/ v
water and filter. To 5 ml of this clear filtrate, add a few drops of
0 n* v7 l% t0 K$ j. }! mhydrogen peroxide; an orange-red colour appears immediately.0 _' M0 C. @$ @$ b8 Y- {: B
PURITY
) W3 F" ^$ q! vLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)4 l* ?" e {0 _5 j4 z ~0 {1 `2 b* t
Loss on ignition (Vol. 4)
h9 l) I* Y" a% u/ `' H9 |6 KNot more than 1.0% (800o) on the dried basis
( \" e7 s* g. ~' wAluminium oxide and/or4 Q' ~- {" A8 z* Y7 G
silicon dioxide$ U2 b' G' s- d% w0 d
Not more than 2%, either singly or combined+ F, D! ]/ X6 i- z) ?! N8 ?$ H
See descriptions under TESTS+ D* a7 ]/ ?- ]7 {0 [
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
$ c" @: c1 Y9 V7 Y. b7 Falumina or silica.& }* O( w) n! w% r
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and0 B) O4 c+ A8 N1 m) D
place on a steam bath for 30 min with occasional stirring. Filter' w a8 P9 J2 L$ u
through a Gooch crucible fitted with a glass fibre filter paper. Wash" r7 b6 R" Z' ~3 o
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the8 R) H) W S `2 y6 X' L
combined filtrate and washings to dryness, and ignite at a dull red
: K& t+ g: d/ l; y" Z8 ?( V, oheat to constant weight.
/ P) i& U/ A4 R5 zWater-soluble matter
* R' u2 r7 d# c! a(Vol. 4)) t5 {. u \# h0 [/ I' v& o
Not more than 0.5%* b- E4 v& g; f$ N- g* o
Proceed as directed under acid-soluble substances (above), using
+ i" o1 S) C% a: |! W* ~$ Mwater in place of 0.5 N hydrochloric acid.
- A" J( `6 e2 E' J3 m, tImpurities soluble in 0.5 N( y, |$ ]- w/ K! w) d, _
hydrochloric acid
* o ~) F9 {* {- y! rAntimony Not more than 2 mg/kg# d7 _, M7 D2 J X
See description under TESTS4 M3 n" Y2 a3 W+ ~! _7 p* h. I6 y
Arsenic Not more than 1 mg/kg
6 P& R) x3 A* Q: l. d! ~( K* J- rSee description under TESTS$ n" f* f, b+ S: a& t) U1 {) V0 ~
Cadmium Not more than 1 mg/kg
0 `- L! \0 f) K' kSee description under TESTS; N/ R' p4 n9 j: j# ?% J
Lead
/ X+ o* l3 E( X+ @: F5 cNot more than 10 mg/kg: y+ w: _/ h9 W9 J( @
See description under TESTS
/ D) [# R0 N5 M0 PMercury (Vol. 4) Not more than 1 mg/kg
8 n% ~+ S* Z. d2 RDetermine using the cold vapour atomic absorption technique. Select a+ P" ]% B) i. G3 ^6 H
sample size appropriate to the specified level% l! K, d3 u, O6 @/ ^- C' \; u* D
TESTS3 d7 ]% n5 n$ f, |% n# D- Y
PURITY TESTS
- p7 _6 y3 G' ^* v+ t0 b+ qImpurities soluble in 0.5 N% E/ B( [. [0 Y8 G8 h! z' k5 ?
hydrochloric acid$ U0 C* _* b5 C0 s
Antimony, arsenic,, K# C1 M7 m; Q) K J
cadmium and lead
- o) T$ B: Z# x+ E& y' h(Vol.4)$ |" \* T5 d' z
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
4 Y2 H6 j! z5 V( \8 O0 q ~& nhydrochloric acid, cover with a watch glass, and heat to boiling on a# W% I0 t O' H R7 f
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
+ W1 \7 }1 M6 l% k1 ]5 z2 K Rcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
) d+ S+ [, E, q- C1 X+ k' l( x* Umaterial settles. Decant the supernatant extract through a Whatman
- F# ^0 e, v/ ]& c1 NNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml; x8 R# o! X5 P! Z3 j! x
volumetric flask and retaining as much as possible of the undissolved
7 L" t0 I& D! F/ Tmaterial in the centrifuge bottle. Add 10 ml of hot water to the original5 n5 c6 G; ^4 m. Q# c6 g t! c
beaker, washing off the watch glass with the water, and pour the
6 I$ G1 m0 g) v0 c! gcontents into the centrifuge bottle. Form a slurry, using a glass stirring
# c! n& Y6 X4 @3 k$ G8 crod, and centrifuge. Decant through the same filter paper, and collect
# `( Y' F1 L1 Athe washings in the volumetric flask containing the initial extract.
2 O/ S6 q1 J4 H( }/ NRepeat the entire washing process two more times. Finally, wash the3 k4 w, E/ w8 R5 n& c
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask* N( ~, D: ^; m6 C
to room temperature, dilute to volume with water, and mix.
6 D% y! R6 J yDetermine antimony, cadmium, and lead using an AAS/ICP-AES' E+ `. e' H9 {; T9 a
technique appropriate to the specified level. Determine arsenic using the
: a. M! w a) b/ f" G$ T J" VICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
3 O% k6 b; y* L: _Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
9 V- s3 a9 ~ {$ n; O/ p8 t* w1 g. The selection of sample size and method of sample preparation
i0 p( {8 n u0 C$ I+ u( h0 amay be based on the principles of the methods described in Volume 4.4 c/ u+ {! u& I6 d. J) W3 a; P
Aluminium oxide Reagents and sample solutions* E" d0 k: x/ j9 |, A) b
0.01 N Zinc Sulfate9 S* ^9 e. r+ t* O6 ]" T" j
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
. V- f- F' V& D2 ^make 1000 ml. Standardize the solution as follows: Dissolve 500 mg8 T3 y- i% I" C, ~* F3 U5 t9 f2 k
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of0 g9 x4 K# e# n8 a
concentrated hydrochloric acid, heating gently to effect solution, then
0 l" w, B+ L7 b7 G# M4 Y, Q8 _transfer the solution into a 1000-ml volumetric flask, dilute to volume
& @4 Z; j; a4 S6 kwith water, and mix. Transfer a 10 ml aliquot of this solution into a 5000 I2 x. m2 U% d- N3 r$ j
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
" c( M6 S Y# A) T* N7 m* Kconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
F: y& p$ y+ H8 L2 s25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,$ v- C/ q8 ?, e- n0 D5 v# R
dropwise, ammonia solution (1 in 5) until the colour is just completely5 e, |6 C4 l# H7 c9 P3 Q. Z1 ~0 S
changed from red to orange-yellow. Then, add:) D" m' O$ a4 E
(a): 10 ml of ammonium acetate buffer solution (77 g of
9 L- N1 T5 Q" c& _. e: H# b6 Rammonium acetate plus 10 ml of glacial acetic acid, dilute to
1 y9 E9 @1 l: Y! @1000 ml with water) and
! E. ~$ J& l' ]6 j6 V; x) ](b): 10 ml of diammonium hydrogen phosphate solution (150 g
* c) K. w9 e. {* w+ C, e' A7 t: Rof diammonium hydrogen phosphate in 700 ml of water,. Y, s9 `0 l5 _$ E5 C
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
' N5 a8 R' l& o: A" g" n) Hthen dilute to 1000 ml with water).2 w: f [$ A1 D7 t: `2 r
Boil the solution for 5 min, cool it quickly to room temperature in a
* l' E( i* G/ s b3 Vstream of running water, add 3 drops of xylenol orange TS, and mix.% y0 v8 ^( O/ F" x1 c
Using the zinc sulfate solution as titrant, titrate the solution to the first
5 [, R; s5 l/ E. U5 Zyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:4 A! [( i( _. ?" r* r
This titration should be performed quickly near the end-point by6 F6 K! Y# y* B6 j1 [
adding rapidly 0.2 ml increments of the titrant until the first colour, R( ]$ a$ q! ?6 ~
change occurs; although the colour will fade in 5-10 sec, it is the true
$ p: N% b' [' i: H7 v3 i; cend-point. Failure to observe the first colour change will result in an8 |: c& S4 S* B! W* r; m& Z- g
incorrect titration. The fading end-point does not occur at the second. A: R8 _# H+ N9 ]: c9 ?0 W& O% P
end-point.)6 j0 {, N5 S( K5 {0 Q' @: B8 j
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a Q5 N4 g7 H) h. E; E3 ?
stream of running water. Titrate this solution, using the zinc sulfate: b( `, l" t$ i
solution as titrant, to the same fugitive yellow-brown or pink end-point
" t0 T- Y' X2 S7 ~; G8 ~as described above.8 S" }) J6 e( Z
Calculate the titre T of zinc sulfate solution by the formula: K, @! N5 {4 h+ m% |* _. K% r2 y: q
T = 18.896 W / V% M3 i) a6 I5 P% Q% v' p& m
where
7 N- E5 o( c+ n' Q& v5 W9 aT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
& W! I# l1 Q# d" ?7 \W is the mass (g) of aluminium wire
5 v& U G Y* bV is the ml of the zinc sulfate solution consumed in the
3 X" I5 Z3 d" V# N1 Y8 @second titration
; D' l2 P* J5 @$ ~5 {9 @2 _18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and4 v- m: a3 s" W5 G c
R is the ratio of the formula weight of aluminium oxide to
1 {- Z, C4 E( n0 n, _/ ~/ `$ _# l9 ~that of elemental aluminium.9 Y3 ]. `, m1 x9 c' u" ?. x. z
Sample Solution A% P" n$ Q! C7 i$ `6 B# L
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
" k2 S$ i& o/ H/ w5 A; ~glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
% N! ~7 Y8 U. ?3 b/ x* z(Note: Do not use more sodium bisulfate than specified, as an excess
: u* Y- K) b$ n/ ]3 C; oconcentration of salt will interfere with the EDTA titration later on in the
7 U8 a$ y4 g- }' F2 _procedure.) Begin heating the flask at low heat on a hot plate, and7 S$ T# Q$ m- U) ]; A3 \8 s
then gradually raise the temperature until full heat is reached.
3 G$ f2 t! Z% P8 s% c8 u9 u(Caution: perform this procedure in a well ventilated area. ) When
3 j+ H* J+ V9 _$ x; h: hspattering has stopped and light fumes of SO3 appear, heat in the full. \: F0 U' o% L: e& v- m' r
flame of a Meeker burner, with the flask tilted so that the fusion of the
# \0 k5 K* `( U! nsample and sodium bisulfate is concentrated at one end of the flask.
2 m2 r6 c& Y @, aSwirl constantly until the melt is clear (except for silica content), but" [/ d9 F" [" E. r1 T- Q2 v
guard against prolonged heating to avoid precipitation of titanium$ I* B; ]) Y" ^ ?
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
7 L+ P: n9 l9 i+ q0 i5 bthe mass has dissolved and a clear solution results. Cool, and dilute to
0 ^* ~! e) b6 ^( v120 ml with water. Introduce a magnetic stir bar into the flask.
) {+ U+ v. [% G4 M u9 X6 T' lSample Solution B
9 p, B+ |1 w# D5 a- D. {" C. [Prepare 200 ml of an approximately 6.25 M solution of sodium1 F1 P) X/ f* Z! q2 ^) m
hydroxide. Add 65 ml of this solution to Sample Solution A, while
% k, R* i! K% X$ G e, @stirring with the magnetic stirrer; pour the remaining 135 ml of the7 G( L& W; X) E# [1 h8 @$ N
alkali solution into a 500-ml volumetric flask.1 n. r0 u& a( G! h7 \1 ~& k5 E
Slowly, with constant stirring, add the sample mixture to the alkali
. s& @5 q! A) E" [/ h6 i2 Ysolution in the 500-ml volumetric flask; dilute to volume with water,5 o$ ^( r+ v( \
and mix. (Note: If the procedure is delayed at this point for more than) C5 k: w+ ^7 P' \0 j& m8 m. d9 z
2 hours, store the contents of the volumetric flask in a polyethylene
& d) R' g% B8 ]! e2 Cbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
1 E e# H- `2 _8 m% K* Zthen filter the supernatant liquid through a very fine filter paper. Label1 \/ r1 _" p& o. D, f) T
the filtrate Sample Solution B.) h* c/ ?* x3 Y C6 t
Sample Solution C& X0 [1 a' A& D" z' b) l
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer3 V: m" ~" ]; ~! j' x8 P5 a; ~
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid: e. @0 y7 v5 r- H) s
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
9 ~1 Y/ f' z2 T' Y0 O6 ^/ ]- xM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is( G" b5 ]! p7 g' x f
known, calculate the optimum volume of EDTA solution to be added
. n; w- Q' g* k/ [) \% s5 Hby the formula: (4 x % Al2O3) + 5.]
* v4 R, _7 A( h) m& RAdd, dropwise, ammonia solution (1 in 5) until the colour is just
% c8 N- p& N& Y6 `4 R' E& mcompletely changed from red to orange-yellow. Then add10 ml each
& `8 H5 O( i% iof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
8 E$ D5 p B0 S+ V9 j: q" ?room temperature in a stream of running water, add 3 drops of xylenol9 @3 h( B: ~' a5 ]+ q$ _- m
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
) [2 N; E9 s: Dbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
: S$ b5 F% F$ v lpH, a pink colour indicates that not enough of the EDTA solution has
2 h, A* e! G6 V/ K/ L) pbeen added, in which case, discard the solution and repeat this
* C( T6 N8 @) f8 X) C# |- h4 L3 Cprocedure with another 100 ml of Sample Solution B, using 50 ml,- v+ s7 n! E# w# n& C
rather than 25 ml, of 0.02 M disodium EDTA.
' Z$ v# {9 a/ q) [, `9 E! O2 _Procedure
( S: B. W2 G' dUsing the standardized zinc sulfate solution as titrant, titrate Sample
# t& V5 S$ o1 q5 m/ B) e4 ?: X3 MSolution C to the first yellow-brown or pink end-point that persists for
- L* `. M! @/ d4 G5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
: h8 U& E' H8 q3 ]4 E. K! Ytitration should require more than 8 ml of titrant, but for more accurate
: i" E2 s9 x% n4 { wwork a titration of 10-15 ml is desirable.4 E/ \( C3 \1 b7 y6 X% V
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5" C. ?, Y; k- p" a
min, and cool in a stream of running water. Titrate this solution, using% T& ^: E3 \; K9 F
the standardized zinc sulfate solution as titrant, to the same fugitive, l" K* Y$ G# o, B1 r- J/ z# Y6 \5 P
yellow-brown or pink end-point as described above.
2 B2 C* j" a9 V" iCalculation:0 t# u+ |0 ]5 Z( n$ y) E
Calculate the percentage of aluminium oxide (Al2O3) in the sample
0 w. i% u, F& C" x" u% v2 mtaken by the formula:& D. M9 Y" q# W8 e' T6 q
% Al2O3 = 100 × (0.005VT)/S
# \. d% Z, t0 n; Kwhere
3 k3 r# ~/ S3 @2 _4 WV is the number of ml of 0.01 N zinc sulfate consumed in
K2 r+ Q! i; C G9 o- Pthe second titration,
( S4 {6 E% h) A3 }9 g3 Y0 NT is the titre of the zinc sulfate solution,. F. h' t7 R) p" D
S is the mass (g) of the sample taken, and: Z0 J) y5 A" X4 |/ u, f
0.005 = 500 ml / (1000mg/g × 100 ml).
( ?3 l# _" Q3 m+ @/ r; pSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
3 v: g: H! t+ V9 |4 N7 e Oglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
7 O. ` r6 q. y! ^Heat gently over a Meeker burner, while swirling the flask, until- e* z" [7 m) ?
decomposition and fusion are complete and the melt is clear, except& z9 a m# p0 D1 d& Z: b
for the silica content, and then cool. (Caution: Do not overheat the4 ?. c" G# z! C- d
contents of the flask at the beginning, and heat cautiously during5 d: T) K' c& p! P
fusion to avoid spattering.)+ P$ }5 k( y3 O" [' _0 [
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
3 p `/ S% E/ l" I5 l$ pcarefully and slowly until the melt is dissolved. Cool, and carefully add
$ u! {# Y1 E" k! f7 }150 ml of water by pouring very small portions down the sides of the
$ u) I9 u+ x% ~flask, with frequent swirling to avoid over-heating and spattering. Allow& a ~% N2 f% M4 z9 S
the contents of the flask to cool, and filter through fine ashless filter2 j7 J, C/ w) e0 I) b# G
paper, using a 60 degree gravity funnel. Rinse out all the silica from
& N! ?. R: ], I/ D- C" Nthe flask onto the filter paper with sulfuric acid solution (1 in 10).
* X, b9 E, ^& `+ }" I! ~Transfer the filter paper and its contents into a platinum crucible, dry in
1 y, A' E. | a$ [+ f- `an oven at 1200, and heat the partly covered crucible over a Bunsen0 H2 U, p( v5 f( v
burner. To prevent flaming of the filter paper, first heat the cover from
. t' O* o6 U/ sabove, and then the crucible from below.
; C1 `/ i) V; zWhen the filter paper is consumed, transfer the crucible to a muffle/ Y3 t3 N! x( {3 M7 w
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
& P b: j# }2 q! wweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated, } ]5 B4 Z0 c! V, e6 }2 x
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first* R, R) A! R( ?# [/ K: `1 s
on a low-heat hot plate (to remove the HF) and then over a Bunsen" R/ a) u% j: d9 B$ L
burner (to remove the H2SO4). Take precautions to avoid spattering,
) h" ^5 V; g4 {. [5 p& kespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
1 M6 h9 H- i( k/ k6 b- k9 T" hdesiccator, and weigh again. Record the difference between the two3 A% c& i( W( z1 P5 W( p
weights as the content of SiO2 in the sample.. j, h& o" }9 x' `7 H
METHOD OF ASSAY( L! I: h W% @7 h0 i/ ^- s
Accurately weigh about 150 mg of the sample, previously dried at 105o
& u( D9 S$ T8 o* sfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water+ D- q- t, d- y
and shake until a homogeneous, milky suspension is obtained. Add 30
}; f/ h1 Y8 G# ], m! K2 Qml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially6 c4 h* c6 n6 I! z# u0 C$ Q
heat gently, then heat strongly until a clear solution is obtained. Cool,( g' C, T- h8 |0 Z
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric5 w9 D+ |- h& |0 x+ Z& T- \' p
acid, and stir. Add 3 g of aluminium metal, and immediately insert a1 N$ y( n; w! t$ L. {
rubber stopper fitted with a U-shaped glass tube while immersing the
/ v3 ]5 b& i6 k& }; Iother end of the U-tube into a saturated solution of sodium" N: ?$ [& l' R. o
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
/ Y' Q. t1 O4 Y+ i$ \hydrogen. Allow to stand for a few minutes after the aluminium metal
0 H) e: e. m9 v- ~7 Bhas dissolved completely to produce a transparent purple solution.
! o/ ~# _( g5 mCool to below 50o in running water, and remove the rubber stopper" f4 @. Z; q0 d. W
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate+ ]0 t$ W+ v# n5 H2 M$ U% B4 O
solution as an indicator, and immediately titrate with 0.2 N ferric- [" @$ L! Z1 x$ U5 M; z& h
ammonium sulfate until a faint brown colour that persists for 30& n- j: O! T. r7 r! e7 f# G8 ~3 ^
seconds is obtained. Perform a blank determination and make any
+ P! {( Q6 e3 F# }* A V2 @necessary correction. Each ml of 0.2 N ferric ammonium sulfate is; C2 s, @+ w: s3 L* I* p
equivalent to 7.990 mg of TiO2.' n, d1 E0 S1 H% ?
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