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发表于 2008-5-23 12:10:00
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二氧化钛(钛白粉)
二氧化钛(钛白粉)
, B9 |3 T; _1 |" E. D# v: K6 k& [- o( G6 \( u5 y d
JECFA关于二氧化钛(钛白粉)的结论5 k% ~5 Q) Q% W# D: }# @5 J
H$ O2 Z( O! t8 v4 }6 @/ e" ~摘要: 2006年JECFA关于二氧化钛的结论2 M% I6 t+ y0 H9 q8 A# ^
ADI值:不作限制。: |- A4 |& u3 o5 p, |$ a
功能:着色剂
$ U" e% b% ]& \+ \/ P5 n* P Q, E' P. q4 o7 |
TITANIUM DIOXIDE, m" m; Q, `5 F% I9 x, n, M& |
Prepared at the 67th JECFA (2006) and published in FAO JECFA3 @$ g" O8 F3 f
Monographs 3 (2006), superseding specifications prepared at the 63rd. o; K# H c7 E# ?, m5 |( P7 i, Z
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
3 h7 W# Y' y6 G Y% {' WCombined Compendium of Food Additive Specifications, FAO JECFA6 G5 s0 H8 Q: t# e+ l9 B/ o9 m
Monographs 1 (2005). An ADI “not limited” was established at the 13th
c0 O- K/ z1 Q0 y; X# b8 V8 {JECFA (1969).; O* P; ]7 a5 f, ^) y. [
SYNONYMS( U9 V6 P7 A2 a6 F
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
+ p0 D: ^6 L+ y/ x& _DEFINITION
! D- v4 @5 e$ w @5 b9 P# @! L* LTitanium dioxide is produced by either the sulfate or the chloride6 }5 {3 C$ M( l+ d& s. g6 {! }
process. Processing conditions determine the form (anatase or rutile
4 T$ T3 ~9 j4 [$ \& ~; istructure) of the final product.
: Y6 K2 a* ~. k9 [! |In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
' z3 I6 d& r) ]or ilmenite and titanium slag. After a series of purification steps, the% z8 I4 n' y% [) d2 y' [
isolated titanium dioxide is finally washed with water, calcined, and" A7 x% m0 T @' s
micronized." t: N" ]6 V7 _7 V% d
In the chloride process, chlorine gas is reacted with a titaniumcontaining
4 n8 j" `- m1 g2 ?; S R' c3 umineral under reducing conditions to form anhydrous
* B0 S; j; g |0 }titanium tetrachloride, which is subsequently purified and converted to
5 |6 w* U5 n' C8 C" W3 h) ltitanium dioxide either by direct thermal oxidation or by reaction with+ I+ P. }- S; E4 x9 P2 F4 f
steam in the vapour phase. Alternatively, concentrated hydrochloric
G9 i6 x4 K( {2 a. Q% cacid can be reacted with the titanium-containing mineral to form a
8 C1 u5 w9 I; z, g0 Q3 h, ~/ ksolution of titanium tetrachloride, which is then further purified and) i8 t' y0 `( M+ J3 }- R: [
converted to titanium dioxide by hydrolysis. The titanium dioxide is/ \6 y4 Q# ~: I' n3 x
filtered, washed, and calcined.
: g% s0 ^5 f8 S* s4 C/ pCommercial titanium dioxide may be coated with small amounts of7 ~' A1 O% m% ?0 j& l k
alumina and/or silica to improve the technological properties of the
$ y5 i% V4 E+ Q+ ^! Uproduct.1 h( W& |+ `+ ?$ ?- _
C.A.S. number 13463-67-7+ @% a1 j! P, B5 j/ d) D, }
Chemical formula TiO2
. _9 p5 {1 p" f; \Formula weight% s0 S- j9 x: E W; M
79.88
7 H* U9 y9 t- m8 h' pAssay
* q# P: X4 ]1 c7 f( w# u8 ?Not less than 99.0% on the dried basis (on an aluminium oxide and
) ^, v; E1 `4 q. \/ Msilicon dioxide-free basis)
1 }; \' N# b& `DESCRIPTION/ H5 p$ k. J3 l
White to slightly coloured powder6 B [+ f* z$ A: A5 I, }/ K
FUNCTIONAL USES2 X) `' _" B+ z3 y; L4 k
Colour
R6 ]3 r" ` T& u0 W0 PCHARACTERISTICS
% \$ O" B& t. [IDENTIFICATION/ |: G( B$ d2 ?3 w/ u& s
Solubility (Vol. 4)4 N9 r0 m- K' X/ i( j
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic t! u: a8 {. C; j) f
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated- X1 {" A$ X, E# D0 J
sulfuric acid.
^9 g6 Z: q5 |9 NColour reaction; h" u% z& Z) y- E
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
b n* C# }: ?* V" Jsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with1 S- ?" S: R1 ~) R& w
water and filter. To 5 ml of this clear filtrate, add a few drops of
1 Y& G! c& b5 Z# Whydrogen peroxide; an orange-red colour appears immediately.8 `% w' j4 `1 ^. Z- ]3 B7 A2 O3 ^
PURITY( j7 q2 A1 Z: z3 V9 e# z
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)% p- ?9 ?" c/ F! U
Loss on ignition (Vol. 4), [" Z; H Y: O1 a. v; I& X/ B
Not more than 1.0% (800o) on the dried basis J( M* X+ v, i$ ^
Aluminium oxide and/or
0 J {/ r# C% Psilicon dioxide
% R5 m3 b: f9 S/ b% b! FNot more than 2%, either singly or combined/ `9 l( R! |( N. _0 K2 J
See descriptions under TESTS
: y" q3 @( y5 k% ~Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
8 |, Y/ v5 R" [' y) ~alumina or silica.1 E! [( B i8 h& n% _
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
& r X" @% p* p7 V9 ?1 vplace on a steam bath for 30 min with occasional stirring. Filter
+ H! o! y8 e" i0 o/ Q2 ?0 gthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
& R# X9 _9 h9 iwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the5 D5 L# M) p' F3 w) M" w
combined filtrate and washings to dryness, and ignite at a dull red9 w5 s, H; `+ y0 i+ M4 ~
heat to constant weight.
6 b# Z" h- S" [Water-soluble matter
) z3 j4 }2 l4 d) g! l2 x' m(Vol. 4)% ]& ]% B$ X- r) v5 O, T1 M: [
Not more than 0.5%
5 r Z3 _) o, `" I2 c9 ]Proceed as directed under acid-soluble substances (above), using3 F+ J2 u! q# I
water in place of 0.5 N hydrochloric acid.4 L0 [) C2 M( B4 o$ f" O) N
Impurities soluble in 0.5 N
- Q+ {* N p/ J- M1 Lhydrochloric acid8 J7 I8 K5 P9 H' l: ?
Antimony Not more than 2 mg/kg
1 M' b; _7 t8 [8 S* O( g/ s9 n; \See description under TESTS
% j3 g3 J- F5 K6 V- CArsenic Not more than 1 mg/kg
/ S+ m% r" ~& [( S- R" m: q* `( ~: @See description under TESTS
2 N, Y% r* @$ B* D; m0 jCadmium Not more than 1 mg/kg
8 x5 W& s6 {6 S1 h' K' x% a1 ]6 pSee description under TESTS1 A% Q/ e) T# R8 Z* l% w
Lead
1 w+ B& l" j& s. G( q1 v SNot more than 10 mg/kg V8 g; Z$ w& Q d7 i. A: B
See description under TESTS
! x' K0 z' R0 r1 ~. h: J! `Mercury (Vol. 4) Not more than 1 mg/kg4 j' n: K6 {; a- l3 d
Determine using the cold vapour atomic absorption technique. Select a
9 N% n# ?+ E/ I- Ksample size appropriate to the specified level
/ R( Z- o8 e1 N+ e8 PTESTS
# I8 a4 n0 I3 I5 D aPURITY TESTS
3 u; u7 q, J- `, d" XImpurities soluble in 0.5 N
2 R2 Y7 B4 i5 ^% q* Uhydrochloric acid
% k6 }. R( Y9 HAntimony, arsenic,6 {/ \9 |5 s% u5 w7 T0 p
cadmium and lead6 a `) a, M3 ~1 c
(Vol.4)
4 b" _6 ]! k3 d: c7 b4 FTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
( k+ Q: E X ^4 f: i1 n, p; A) shydrochloric acid, cover with a watch glass, and heat to boiling on a
" E! t/ l8 E6 @1 z& t, Ahot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml/ H1 t7 w. Q% l- A
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
; `, I2 A" |5 m: C) ?7 o8 tmaterial settles. Decant the supernatant extract through a Whatman/ M: P" A- w+ d$ n( K
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml. y# K* @/ E4 s/ Z8 Y% O
volumetric flask and retaining as much as possible of the undissolved; z1 ~" b5 X4 ^9 u! I
material in the centrifuge bottle. Add 10 ml of hot water to the original0 S% \! O& C d5 {6 d7 l
beaker, washing off the watch glass with the water, and pour the" L* M& M7 p9 i; t" K0 ]$ U( z
contents into the centrifuge bottle. Form a slurry, using a glass stirring
) r/ z# Z" E3 u" G irod, and centrifuge. Decant through the same filter paper, and collect
T% S9 H; i0 k) L) Ythe washings in the volumetric flask containing the initial extract.& q P) d, [+ C) m& c! O7 p6 U
Repeat the entire washing process two more times. Finally, wash the
% `% V/ Y* b0 i: afilter paper with 10 to 15 ml of hot water. Cool the contents of the flask& Z6 U# I. p6 @" Z: `1 U
to room temperature, dilute to volume with water, and mix.
8 r6 _0 o% ^$ w$ k) p$ R$ fDetermine antimony, cadmium, and lead using an AAS/ICP-AES2 w* W; F( G/ p: P0 Z
technique appropriate to the specified level. Determine arsenic using the# n+ L7 `- t- ?" F
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
' k) J* \8 g! ?) jMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
( D8 D4 x t5 y0 T% _1 g. The selection of sample size and method of sample preparation
8 A) N/ n0 O# j! ]9 {may be based on the principles of the methods described in Volume 4.
# F( {- @( v. b* PAluminium oxide Reagents and sample solutions j. g4 c8 t1 s! ^ z- G4 i
0.01 N Zinc Sulfate& v" x& z5 g h; ?6 r* J
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to! [- x( V) Z5 E6 R2 t) Z0 m
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg9 b( W9 f) O) k% [
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of' O" D$ [9 i: a: D3 U& \3 S+ [
concentrated hydrochloric acid, heating gently to effect solution, then( s7 Z5 D0 U/ n7 \; D
transfer the solution into a 1000-ml volumetric flask, dilute to volume% i, r* `& n! c2 L% A
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
: M: {5 K$ o0 R }! R9 zml Erlenmeyer flask containing 90 ml of water and 3 ml of
; T l3 y0 {9 D% [& h, b( fconcentrated hydrochloric acid, add 1 drop of methyl orange TS and2 h1 u$ I5 x+ x
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add, ~# X. s, M9 H! u9 ]% U) [
dropwise, ammonia solution (1 in 5) until the colour is just completely
. {$ S+ `6 N! E' y! echanged from red to orange-yellow. Then, add:
$ Q+ U0 Q2 `* j7 o6 K8 ?. @- Q(a): 10 ml of ammonium acetate buffer solution (77 g of
; d: f9 o* ?4 V9 i" L# kammonium acetate plus 10 ml of glacial acetic acid, dilute to6 D5 j% D4 p$ a( ]
1000 ml with water) and' R, t% M$ V4 ]% ?$ m6 }1 M3 P$ z
(b): 10 ml of diammonium hydrogen phosphate solution (150 g8 h; B* |# N: B2 Z1 ^& t- f W
of diammonium hydrogen phosphate in 700 ml of water,
2 M- O9 t% F8 o8 ^: c* c9 I! Padjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
" I, x0 X* R) @! f1 l6 `2 Gthen dilute to 1000 ml with water).
$ v) |$ z( ^5 JBoil the solution for 5 min, cool it quickly to room temperature in a
; c/ @" x- Q. Nstream of running water, add 3 drops of xylenol orange TS, and mix.* _9 u% Z0 X# k) V0 B) ?- {8 G, }
Using the zinc sulfate solution as titrant, titrate the solution to the first
* K: t1 I- G, s* W( P3 Tyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:4 D4 `5 s3 w' Z: P
This titration should be performed quickly near the end-point by
4 ?0 M( [: M" j5 l5 t7 I! k8 Iadding rapidly 0.2 ml increments of the titrant until the first colour9 ~8 s. G$ o( h* U' Y+ @
change occurs; although the colour will fade in 5-10 sec, it is the true
$ M5 C1 \3 j# y, Z" p! gend-point. Failure to observe the first colour change will result in an8 w- o* V! z- Y3 U3 d9 R& P. @3 U
incorrect titration. The fading end-point does not occur at the second
* i3 _; X. R& O. ]" I# P) y M4 U) I% Send-point.)6 g* b. p3 }5 i/ }0 _
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a+ I2 Y0 [* l$ @" U9 t" j0 Q
stream of running water. Titrate this solution, using the zinc sulfate
/ y8 v2 q8 B _! j$ Y& nsolution as titrant, to the same fugitive yellow-brown or pink end-point
5 J/ _( @6 p# Was described above.# H, J" ]4 @/ e0 Z' J& t
Calculate the titre T of zinc sulfate solution by the formula:
+ ]4 K( [0 V5 g5 k/ {3 ]T = 18.896 W / V) o9 t6 H P: ~/ E! I" m
where
, ~6 D; m r L' }: R4 C! UT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
" N! l1 l; L1 P! [- S; ZW is the mass (g) of aluminium wire
9 x5 A$ u+ Q7 Z& C" qV is the ml of the zinc sulfate solution consumed in the
A2 ~. g2 f) Usecond titration% o+ g) A; D5 R7 h8 F
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
2 y+ ~4 |' ]+ A& U3 |$ N# fR is the ratio of the formula weight of aluminium oxide to1 D) l. x- f/ l1 P) K- I
that of elemental aluminium.: Q( n9 V2 Y w6 h7 o
Sample Solution A
5 h1 Z4 ` P6 m Y& w, kAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica& I, n9 h, y8 P8 h
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).# V( g# K4 y8 G( `( P: ?
(Note: Do not use more sodium bisulfate than specified, as an excess
% D! u* u: B* P5 A3 \concentration of salt will interfere with the EDTA titration later on in the) S, N" A; ~- O& w( i9 Z( d
procedure.) Begin heating the flask at low heat on a hot plate, and) N! s0 o4 V6 x l& S
then gradually raise the temperature until full heat is reached.
+ C% T6 x$ \. S) b& Y( t3 y(Caution: perform this procedure in a well ventilated area. ) When& G5 d5 i* ^: [, M. D, J
spattering has stopped and light fumes of SO3 appear, heat in the full7 `5 Y. P) O& D+ S8 v4 Q c7 @6 |) _
flame of a Meeker burner, with the flask tilted so that the fusion of the
$ Q8 C* f; J2 |" U" t9 Usample and sodium bisulfate is concentrated at one end of the flask.
) V9 d1 O7 e2 U! G7 {5 e5 sSwirl constantly until the melt is clear (except for silica content), but
~: S# W" D, I1 F8 o4 N4 Zguard against prolonged heating to avoid precipitation of titanium
2 G' }; i) J/ U- v' g. {+ ^* sdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until5 s! X/ l# U6 W ~! l7 j
the mass has dissolved and a clear solution results. Cool, and dilute to
8 x/ Z' o) J3 M" G: C7 O; _120 ml with water. Introduce a magnetic stir bar into the flask. e. X' b% a* z7 L
Sample Solution B
8 d: u7 b: w9 gPrepare 200 ml of an approximately 6.25 M solution of sodium9 j+ x A$ N- q- A( N; K
hydroxide. Add 65 ml of this solution to Sample Solution A, while5 ~4 O" b6 w; t$ F2 ]0 ^
stirring with the magnetic stirrer; pour the remaining 135 ml of the
7 T8 _- d: |4 e# q) D7 n2 P: ~alkali solution into a 500-ml volumetric flask.
0 |3 Z# ~9 ~" ~4 m/ {+ m/ BSlowly, with constant stirring, add the sample mixture to the alkali
5 l4 Z1 h( ]7 ?' fsolution in the 500-ml volumetric flask; dilute to volume with water,
. c6 y; z( b2 u: R& L: F" n" yand mix. (Note: If the procedure is delayed at this point for more than
& F& M; q% D, }. h9 s6 r2 hours, store the contents of the volumetric flask in a polyethylene
- D/ o7 |) U; J3 Zbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
! [# j# [" t0 L9 u8 a7 ithen filter the supernatant liquid through a very fine filter paper. Label
& b3 R) s$ C9 Q5 zthe filtrate Sample Solution B.
; W! E; ?* O) ?5 eSample Solution C
) e) n6 ]" _7 ?7 `! A/ n3 c9 _! F8 D/ [Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
8 Y8 u9 e5 ~, W) Q2 w ^4 }flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
1 f; Y2 u( \. y3 R* D2 ^" Gsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
9 Q) b& R, }8 N; O% P3 E8 `9 tM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is- V+ \# _- b' c6 K% Z) ~
known, calculate the optimum volume of EDTA solution to be added
3 X7 t9 M* c1 @6 R4 Q1 ^$ hby the formula: (4 x % Al2O3) + 5.]
' x* v# n$ d8 ]) Z) [% @) C: a9 _Add, dropwise, ammonia solution (1 in 5) until the colour is just
# v; F& \$ P" [5 k l" Bcompletely changed from red to orange-yellow. Then add10 ml each9 K0 Z7 E, e. r
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
- `- f5 G* U6 lroom temperature in a stream of running water, add 3 drops of xylenol- Y- g/ a+ F* V, l
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
8 ?; `! m: l" y; o2 ^bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired( X* w6 m& j; g% R& o
pH, a pink colour indicates that not enough of the EDTA solution has- ? X/ X" U( f. U$ u
been added, in which case, discard the solution and repeat this
; D3 H; D, y% K# I# ^1 I g5 qprocedure with another 100 ml of Sample Solution B, using 50 ml,. d; E3 ?( X& {' |7 z2 @+ K% I
rather than 25 ml, of 0.02 M disodium EDTA.
+ s7 t7 b# U4 \6 R+ T7 K GProcedure
% _- U4 F' \! u- U' rUsing the standardized zinc sulfate solution as titrant, titrate Sample
' [, d6 u* R. m4 B X8 v# G1 h! B' mSolution C to the first yellow-brown or pink end-point that persists for8 y9 M- e* n$ Y. t: R, o
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first) C7 o [, d% ^% X
titration should require more than 8 ml of titrant, but for more accurate
: f% o, j8 s0 b( J+ U `2 [work a titration of 10-15 ml is desirable.+ x% I* f3 b+ y% T6 V5 [8 M/ c
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
, S5 v2 E( S; z! f3 wmin, and cool in a stream of running water. Titrate this solution, using
! o/ h% R! p V6 R9 L# e W( Ythe standardized zinc sulfate solution as titrant, to the same fugitive
; u, q- H* H1 C$ G- Byellow-brown or pink end-point as described above.
5 U4 E% I, {5 z) v3 k6 X3 U; Y5 i# ZCalculation:" o) }" T H& U$ p! L/ t4 l \& e
Calculate the percentage of aluminium oxide (Al2O3) in the sample7 i/ X1 ?2 L9 H7 |
taken by the formula:. h( O( @9 w2 L+ n- t
% Al2O3 = 100 × (0.005VT)/S$ \( G& W$ p/ L+ l1 Q
where/ U5 t5 u$ o7 h% i
V is the number of ml of 0.01 N zinc sulfate consumed in
; D8 S% I) `; [8 Tthe second titration,$ p0 |1 L9 a* O+ k. C
T is the titre of the zinc sulfate solution,0 ^, U6 d9 n- _
S is the mass (g) of the sample taken, and' s; y- c! c$ Q2 y
0.005 = 500 ml / (1000mg/g × 100 ml).' ~2 ?( O1 J: V+ V. M" |+ i5 ]
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica1 e; a5 m/ s5 S6 k
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).1 }) m; |" K9 Q% p2 i
Heat gently over a Meeker burner, while swirling the flask, until
; `7 o- ~5 n6 @3 [# S5 edecomposition and fusion are complete and the melt is clear, except
6 x: b; F' B& t' v/ Hfor the silica content, and then cool. (Caution: Do not overheat the
4 F5 ~3 X3 P6 L# @) X. |9 X0 vcontents of the flask at the beginning, and heat cautiously during
3 C6 G+ l$ E* s" I7 @7 \8 J4 ifusion to avoid spattering.)
8 Z2 C" P2 C6 q# P" K- ] pTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
: y: A1 @$ Q" ^; P. k; R8 ~. u& |) e% vcarefully and slowly until the melt is dissolved. Cool, and carefully add
Z! V( Y! |+ D) k150 ml of water by pouring very small portions down the sides of the+ w# a1 v- m$ q
flask, with frequent swirling to avoid over-heating and spattering. Allow
( b' x) l, m4 B9 X/ b8 O% pthe contents of the flask to cool, and filter through fine ashless filter
8 z$ H! L& d- ]" D; T( H; upaper, using a 60 degree gravity funnel. Rinse out all the silica from
" F. G/ K U1 b: b; wthe flask onto the filter paper with sulfuric acid solution (1 in 10).
. |- Y3 U% ?/ l N: }1 v) g- |7 DTransfer the filter paper and its contents into a platinum crucible, dry in5 c+ w8 e" p) \/ |/ K6 F h! ?
an oven at 1200, and heat the partly covered crucible over a Bunsen
2 H7 N7 G$ m" \burner. To prevent flaming of the filter paper, first heat the cover from$ R7 C2 z- z$ ]
above, and then the crucible from below.
8 b; N' h# g7 L) A! z% C- u7 nWhen the filter paper is consumed, transfer the crucible to a muffle
0 B" J/ |* I/ ~1 w$ tfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and7 p, V" W" `5 { \% b1 V
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated0 c' u e2 |) c" N4 f
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first/ i. I& }* g Q8 I
on a low-heat hot plate (to remove the HF) and then over a Bunsen
e1 j+ x5 u6 e) O) T0 N Pburner (to remove the H2SO4). Take precautions to avoid spattering,
+ b) \7 H4 G' O# e+ l Hespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
) A& }' ?, b. h! z; M5 bdesiccator, and weigh again. Record the difference between the two3 @3 ~$ Q& l# z) o; b1 Z
weights as the content of SiO2 in the sample.& |/ Q) H, k- W+ Z
METHOD OF ASSAY
$ G% {1 b/ [" x" W1 IAccurately weigh about 150 mg of the sample, previously dried at 105o; i. ]; \: J# J) R# k" ]9 T
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
' q" J, V/ B" }4 N& H" M1 Cand shake until a homogeneous, milky suspension is obtained. Add 30
" C" ~' c8 l8 B2 d* w9 eml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially: K% `3 b: E9 R
heat gently, then heat strongly until a clear solution is obtained. Cool,: h) z) p: h- D
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric: j5 o7 u# u, \6 b) n2 `: ~ z. s+ z
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
) M7 ~, i( K! xrubber stopper fitted with a U-shaped glass tube while immersing the
3 J; R9 {" h$ ~ M, hother end of the U-tube into a saturated solution of sodium
. p/ }, ]- V1 tbicarbonate contained in a 500-ml wide-mouth bottle, and generate
" y& A1 G4 e2 o* whydrogen. Allow to stand for a few minutes after the aluminium metal, i; N5 D4 |9 l; ^: N
has dissolved completely to produce a transparent purple solution.
: @8 H+ ?- H1 X+ n8 O+ D2 qCool to below 50o in running water, and remove the rubber stopper
2 z4 Z/ t+ g& h2 |carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate9 z& X/ O, f4 u( |; t
solution as an indicator, and immediately titrate with 0.2 N ferric7 b3 @' ^, D8 X1 D" ?2 G
ammonium sulfate until a faint brown colour that persists for 309 H: p9 {- y |0 s5 m/ }
seconds is obtained. Perform a blank determination and make any5 w% i% ~& x5 S: Z+ [" C
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
' V4 G* ?; z7 F; W5 M* Qequivalent to 7.990 mg of TiO2.; J2 i% P; r; b' F
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