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二氧化钛(钛白粉)
二氧化钛(钛白粉)4 @- G- C# E$ G) H" ~
+ j% [# V" S3 ^4 ]. Q% P3 lJECFA关于二氧化钛(钛白粉)的结论
2 ^1 Q5 O+ n. H7 j7 e6 O2 C0 q+ w6 d
摘要: 2006年JECFA关于二氧化钛的结论4 p, m S4 L4 F) ^
ADI值:不作限制。
$ b# y. ^: U. r: ~4 x! V功能:着色剂
& d2 ]4 u9 \6 Z/ K& b5 V# t$ n, G4 V( {- ?5 t! J+ z
TITANIUM DIOXIDE
3 a0 [& h( d# T& vPrepared at the 67th JECFA (2006) and published in FAO JECFA/ w3 s2 D5 ?/ w: E4 l1 N: E
Monographs 3 (2006), superseding specifications prepared at the 63rd
% i) g: I6 M8 _& X4 ^5 ?3 rJECFA (2004) and published in FNP 52 Add 12 (2004) and in the2 _- ~) s- a6 B
Combined Compendium of Food Additive Specifications, FAO JECFA1 _7 U4 z# m8 ^: [
Monographs 1 (2005). An ADI “not limited” was established at the 13th
* e: ~9 Z: w; _2 `6 p) t8 dJECFA (1969).
* J3 G. l3 @8 f3 e5 g7 @SYNONYMS# J- @0 B! F9 h# Y; B+ S5 f5 r
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171( k5 e' K3 U- E. d8 y
DEFINITION8 Z8 p' d5 O3 {% P' C0 p
Titanium dioxide is produced by either the sulfate or the chloride
- V O% S2 M: e. Z0 c- b0 f$ Gprocess. Processing conditions determine the form (anatase or rutile
9 T4 m3 y1 R# M* I" t$ ~- estructure) of the final product. t" B4 I3 g1 |- |, R
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
) Z6 W. P% r$ O9 _( z. xor ilmenite and titanium slag. After a series of purification steps, the- E$ t/ O' H2 \% U' g/ z6 `" x
isolated titanium dioxide is finally washed with water, calcined, and- R+ ^' `1 u/ i. z9 Y
micronized.% }" K) D* ~) w' v5 f% d4 A
In the chloride process, chlorine gas is reacted with a titaniumcontaining
) V4 ^& U+ H# r1 V' t* smineral under reducing conditions to form anhydrous
+ \' x- t( l% P% n: W: D. I5 Gtitanium tetrachloride, which is subsequently purified and converted to
, S( q9 }* t1 \: K# xtitanium dioxide either by direct thermal oxidation or by reaction with
+ x5 g+ D. c; }3 _ A( xsteam in the vapour phase. Alternatively, concentrated hydrochloric/ Z! N) b0 X% i) I5 P. k, D
acid can be reacted with the titanium-containing mineral to form a
# j0 I: T' C2 X+ C+ Tsolution of titanium tetrachloride, which is then further purified and
# u# D$ I& E% Z9 l. g) ~converted to titanium dioxide by hydrolysis. The titanium dioxide is& L: k; \, Y* u9 {
filtered, washed, and calcined.
9 d5 d2 T$ K; y8 m7 {' OCommercial titanium dioxide may be coated with small amounts of) I/ X1 R+ E) `! m% {$ I
alumina and/or silica to improve the technological properties of the
' a3 f$ O% ^+ K9 m' q& a' n5 [4 sproduct.' _* I* y; s0 C, _- i
C.A.S. number 13463-67-7
' s8 V) @: [1 R qChemical formula TiO2
6 o$ U: J8 G; B# W- }6 dFormula weight; k! ?: s R; [
79.88
1 G& f/ L8 e- i6 q6 l2 M& U+ `Assay
; _# h6 l8 S% D9 XNot less than 99.0% on the dried basis (on an aluminium oxide and
# d8 P. W. s! R0 I9 Usilicon dioxide-free basis)% q6 O0 s& b0 I, r/ Y3 N: t
DESCRIPTION
3 Y9 s6 g: M2 ~( e) `White to slightly coloured powder
8 A9 @7 i* N) j8 KFUNCTIONAL USES
$ b3 y% G/ Q3 r8 cColour
- O' `5 @# h9 c- J% z. uCHARACTERISTICS; T: W9 z* r3 w5 o v; m
IDENTIFICATION8 {& p) j' w! C7 G% T! \
Solubility (Vol. 4)
5 B, c" D" O& x8 GInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic1 T+ L1 {4 H; U4 w- h% i, k- y' b
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
% ~3 ]4 k) I- Osulfuric acid.
% `3 j G9 K) C. M0 gColour reaction/ P V/ Z$ A/ _( m9 a; \7 Q9 X
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
( ~, r+ I/ E# x; \) l9 o7 ~( Isulfuric acid appear, then cool. Cautiously dilute to about 100 ml with+ i2 x, q. V7 c4 b, H
water and filter. To 5 ml of this clear filtrate, add a few drops of
9 }0 N# t$ O% m0 m5 [! ehydrogen peroxide; an orange-red colour appears immediately.
/ v: V; ]7 b4 h: ~0 H( Y0 u& j) lPURITY+ \. ?9 F5 ]( t4 P$ ^8 b
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
4 A9 F& C. o6 A9 @, M/ pLoss on ignition (Vol. 4)
0 J% R% r# _' G5 g6 ~& INot more than 1.0% (800o) on the dried basis
- F: p2 r* s( C$ l+ Y: LAluminium oxide and/or2 v" S! \8 J1 g, u! V
silicon dioxide1 O: V4 T* v6 c4 i
Not more than 2%, either singly or combined3 |" x. \: g( p1 C' E4 Z
See descriptions under TESTS
1 |, ` A5 Q% g9 |' @* i) A) YAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
/ f9 D( y% y6 [- W- m: j+ P4 L) ralumina or silica.
7 ^% R m% ~" D9 R; k6 \Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and4 n! l, ^8 ]0 x: _/ r2 @! c3 q
place on a steam bath for 30 min with occasional stirring. Filter* t0 K& y+ y; w" D
through a Gooch crucible fitted with a glass fibre filter paper. Wash
. t' q5 \8 j: V( D+ iwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the/ \3 f* t6 E: ]6 h) C) p9 a
combined filtrate and washings to dryness, and ignite at a dull red
/ A8 q. Q, H8 o) R6 w' Xheat to constant weight.
9 Q F( K" m' F6 }! z: u$ i/ eWater-soluble matter
3 E, g$ {0 O' E/ m(Vol. 4)
/ d& q) |, L; S3 e: |- v5 {7 KNot more than 0.5%
0 d0 ^/ A2 b% [+ M) N" B& Q( ^* `Proceed as directed under acid-soluble substances (above), using; G W3 l+ V) f$ ]
water in place of 0.5 N hydrochloric acid.
: }$ U5 ^0 u9 R0 kImpurities soluble in 0.5 N0 N; p9 A1 M. ^3 m% I4 m
hydrochloric acid6 U: `( t+ Z5 s. K J h6 T
Antimony Not more than 2 mg/kg
) D7 |" T# R2 R: o# f' xSee description under TESTS
1 e% m$ J% S1 J$ u! e# X, m2 MArsenic Not more than 1 mg/kg9 m- Q9 |; `0 M& V+ y3 p7 d
See description under TESTS9 Y+ U, a, j2 r7 ^4 D% _7 G
Cadmium Not more than 1 mg/kg
# N# M3 k0 g2 h1 c& C: E2 @( J( eSee description under TESTS) x- _ s- a$ m0 s, a g4 q2 D
Lead- h+ e! n6 `+ K" ^
Not more than 10 mg/kg
: V; b1 q. n: I, |See description under TESTS
& ~2 B2 R/ Y5 E% g2 R3 T' MMercury (Vol. 4) Not more than 1 mg/kg
Y r* o9 E' t9 r6 vDetermine using the cold vapour atomic absorption technique. Select a+ z+ K# D' P, l$ K# O% H
sample size appropriate to the specified level* l b+ G$ l6 o. b2 D' Z
TESTS2 u, J2 M8 ~! E
PURITY TESTS1 D* w3 ]8 I6 X- D- m
Impurities soluble in 0.5 N; h9 _: v# ~% ^. T
hydrochloric acid
; v9 E( l& f, r9 ~Antimony, arsenic,
[9 U9 ]6 U1 y* n7 [* K9 S3 bcadmium and lead
, v' ?$ W! @+ p9 u(Vol.4), k( G) `! v. Y/ H5 {
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N- P5 S3 K% _/ I0 n2 E K! s; W
hydrochloric acid, cover with a watch glass, and heat to boiling on a
3 t& S- Z) R' a( ~: z1 y$ {hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml/ s" m/ U- i; d. J- g
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved2 p4 I' q! l+ O7 v2 h! r2 k
material settles. Decant the supernatant extract through a Whatman) U. p8 a8 O2 ?" Z
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
& b( z5 Y8 K. xvolumetric flask and retaining as much as possible of the undissolved
6 ?; g5 q' ?' a |: c8 A: x" v* Xmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
7 s8 } m) m. N& v8 H! Zbeaker, washing off the watch glass with the water, and pour the
: u! i7 E3 d4 ^8 Fcontents into the centrifuge bottle. Form a slurry, using a glass stirring# T1 c/ K; l( z" s
rod, and centrifuge. Decant through the same filter paper, and collect8 F1 j. s- P( Z) M: B
the washings in the volumetric flask containing the initial extract.
2 C/ G# v% B) p4 G4 p, O! ]5 P ARepeat the entire washing process two more times. Finally, wash the
+ f* d' B. |- A5 ], q: b) |+ o7 @filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
$ O" V: N: ? O1 w# g) G- J. Dto room temperature, dilute to volume with water, and mix.% Z# l9 T- H* |" K0 c& O
Determine antimony, cadmium, and lead using an AAS/ICP-AES# Y9 Q+ Q# ^0 o0 n
technique appropriate to the specified level. Determine arsenic using the
# ]( I1 z- B% a5 U1 {4 s! YICP-AES/AAS-hydride technique. Alternatively, determine arsenic using3 k3 Y, z1 E. W% B2 P/ z
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
% w$ {, X# f% h3 O! f @1 g. The selection of sample size and method of sample preparation( f; x6 E! Q( o' V
may be based on the principles of the methods described in Volume 4.
- m g+ k0 B& H; u. H7 q/ p; fAluminium oxide Reagents and sample solutions, N5 p3 B4 J1 n6 x: L7 p$ ?
0.01 N Zinc Sulfate
0 R y8 {+ F7 W: Z8 rDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
6 n V4 @* v: G' a Wmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg9 c; R6 Q+ g$ d) a! f1 U
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
1 y; s! w% c( econcentrated hydrochloric acid, heating gently to effect solution, then
7 s; ~: C4 I) q0 K! L& C: x1 |# htransfer the solution into a 1000-ml volumetric flask, dilute to volume4 s) w# Y! H9 `% I2 z: f
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500" L, M1 ]: \: H4 U
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
2 F6 P8 f1 _8 ^2 F) @concentrated hydrochloric acid, add 1 drop of methyl orange TS and7 @% e% a, b# i T+ |' s" b
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,0 x) o$ U3 Z- n" S
dropwise, ammonia solution (1 in 5) until the colour is just completely. r: E2 ~" H: E
changed from red to orange-yellow. Then, add:( `# H) Q4 @+ K0 M1 o# D9 R/ @
(a): 10 ml of ammonium acetate buffer solution (77 g of/ {2 B1 s" h g6 y8 |) D; x% M
ammonium acetate plus 10 ml of glacial acetic acid, dilute to( I4 n2 [1 J; s! D4 y
1000 ml with water) and
' T* f6 C' g! d# ] X(b): 10 ml of diammonium hydrogen phosphate solution (150 g" ^( q* |' ~3 X- ]2 ^7 |
of diammonium hydrogen phosphate in 700 ml of water, S0 {0 h4 P" i0 K+ \ q
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,5 X% X3 Y, d- n/ m
then dilute to 1000 ml with water).2 k0 v. Z, F$ N1 N8 f. R
Boil the solution for 5 min, cool it quickly to room temperature in a
! }& B2 C4 L. ]0 x0 ?/ H: Q& ?stream of running water, add 3 drops of xylenol orange TS, and mix.. o% W( p3 o0 }, z3 Y6 N4 ~
Using the zinc sulfate solution as titrant, titrate the solution to the first* F4 C' u6 t/ F8 \) m; G
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:: [% c' c0 l9 i0 T4 ?
This titration should be performed quickly near the end-point by
0 k* r* A/ _( m* c Zadding rapidly 0.2 ml increments of the titrant until the first colour
# O, x8 [9 }; M* u3 J8 ?5 m1 D- {' Xchange occurs; although the colour will fade in 5-10 sec, it is the true
3 S2 h7 D1 N5 t$ N" ?" c5 bend-point. Failure to observe the first colour change will result in an
* V/ S$ L* l3 r3 \7 v* g6 oincorrect titration. The fading end-point does not occur at the second
& J( i3 {9 ] M4 E8 bend-point.)
1 Y7 M/ I: j+ ~4 `6 q" r3 @3 M# oAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
$ u$ \! [" t; e. Vstream of running water. Titrate this solution, using the zinc sulfate G. R: y( T) j
solution as titrant, to the same fugitive yellow-brown or pink end-point+ A( n# O1 i! l% ?7 a$ c( {
as described above.. P* @) D8 y9 O ~( i( j# `+ d
Calculate the titre T of zinc sulfate solution by the formula:# N- I' o6 W, f( F, K% D' H$ F/ r
T = 18.896 W / V
( b' r( d. ^: I. p/ wwhere
N" H7 ]4 ?4 E, |T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
$ k5 u& [4 E6 ]W is the mass (g) of aluminium wire+ n( M/ E! G3 z9 p. P# I' y. K. ]
V is the ml of the zinc sulfate solution consumed in the
/ ~6 c7 Z- e8 V0 N# q2 g1 ~second titration$ n# K; h- ]) r- }$ m$ `9 S
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and$ ?' Z1 S$ U/ y! w' s
R is the ratio of the formula weight of aluminium oxide to
; P! d& Z& b) V8 t6 P% vthat of elemental aluminium.
* V* e6 `+ c1 }% pSample Solution A
0 h1 }' j3 s1 e+ L( u) L7 LAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica( }. G, `5 E( \, K0 W) t
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).* Q9 R/ ~7 p( `
(Note: Do not use more sodium bisulfate than specified, as an excess
/ f$ m" W3 B. ]9 M) O k6 u. iconcentration of salt will interfere with the EDTA titration later on in the% k2 G0 h3 _3 Q+ A* _; [
procedure.) Begin heating the flask at low heat on a hot plate, and
. o6 i" Q9 C+ Bthen gradually raise the temperature until full heat is reached.
2 o6 O$ t8 v1 t1 b a% R(Caution: perform this procedure in a well ventilated area. ) When8 H4 X* y0 `$ O
spattering has stopped and light fumes of SO3 appear, heat in the full
, a2 D9 z8 K( `3 X) t7 H! Z6 vflame of a Meeker burner, with the flask tilted so that the fusion of the
) ?( }% A) x6 G. csample and sodium bisulfate is concentrated at one end of the flask.! r: g: z& _, B8 u1 z0 Y! F
Swirl constantly until the melt is clear (except for silica content), but: h6 ~8 X9 U! v' H" h2 g$ k7 U! F
guard against prolonged heating to avoid precipitation of titanium
! v9 v2 v: X- v$ U7 ldioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until4 E. u& g; U: Z
the mass has dissolved and a clear solution results. Cool, and dilute to
f* X7 j8 i& Q& R% M5 E120 ml with water. Introduce a magnetic stir bar into the flask., v+ u" U, |6 n- }) I2 S
Sample Solution B1 W5 ~( f$ b+ J
Prepare 200 ml of an approximately 6.25 M solution of sodium; |& M$ g0 E6 Z" g
hydroxide. Add 65 ml of this solution to Sample Solution A, while
; R8 K' j" l# ^5 _/ Kstirring with the magnetic stirrer; pour the remaining 135 ml of the
- n2 S+ l9 _: `$ Zalkali solution into a 500-ml volumetric flask.
' Y( E Y+ `; E# z3 dSlowly, with constant stirring, add the sample mixture to the alkali
8 p O( g# S; xsolution in the 500-ml volumetric flask; dilute to volume with water,% L- S& T- n+ ~& u0 q1 ~ c* v
and mix. (Note: If the procedure is delayed at this point for more than
/ s' O5 k. A( k/ ~ f2 hours, store the contents of the volumetric flask in a polyethylene; ]% Q, R t* i" Y8 _$ h
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
1 H/ Q3 o0 n }0 O+ P+ mthen filter the supernatant liquid through a very fine filter paper. Label, N% L( \# k; q. e/ h4 q
the filtrate Sample Solution B.
, Z% R0 U$ D9 m! u# {: ~2 eSample Solution C7 A; y! f: o; u! D% j
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer, K1 x1 G1 x) C+ }' U
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid( q1 k$ z U1 O0 @& [. Y
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
* r- |# `9 Y: FM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is" v6 G7 [3 p1 c' {
known, calculate the optimum volume of EDTA solution to be added: o& S" d- A: z. w+ w% ^5 L/ G0 V5 F
by the formula: (4 x % Al2O3) + 5.]3 \ X6 j! g1 G$ G$ h5 e
Add, dropwise, ammonia solution (1 in 5) until the colour is just) }! y' E) j6 c+ h
completely changed from red to orange-yellow. Then add10 ml each5 ]9 Q3 \" P; G) l9 n/ x
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to% l9 K: i$ D f% ^# b$ t& l
room temperature in a stream of running water, add 3 drops of xylenol4 v0 N) F3 o$ c) W. d+ \
orange TS, and mix. If the solution is purple, yellow-brown, or pink,% J2 {9 Z. S$ E# M
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired y1 ]- g5 F3 C% y1 H
pH, a pink colour indicates that not enough of the EDTA solution has
" A* Y& Y& e& w* W; N5 D( n4 @been added, in which case, discard the solution and repeat this
. M' c5 U0 a9 q4 ]' J- b1 Fprocedure with another 100 ml of Sample Solution B, using 50 ml,- `; j) l; o8 B8 ^
rather than 25 ml, of 0.02 M disodium EDTA.
, w6 ?, Q: m" p, LProcedure$ t2 l0 ^# ^% B, r- e( F
Using the standardized zinc sulfate solution as titrant, titrate Sample9 X- ^' I+ A n
Solution C to the first yellow-brown or pink end-point that persists for
0 }0 D, Q0 y( f0 F) ~& e5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first$ }7 |5 H: f$ A9 X5 T* {
titration should require more than 8 ml of titrant, but for more accurate
" i5 O) `2 x% k1 O+ ~& `work a titration of 10-15 ml is desirable.
7 d9 c/ _& {1 w: |5 P1 V' {Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5+ V# |" `0 h2 ]0 k
min, and cool in a stream of running water. Titrate this solution, using# P1 c1 D7 Z0 o. a8 [, v
the standardized zinc sulfate solution as titrant, to the same fugitive
, ?* m* I# l3 b) S3 I3 |, D$ T% ryellow-brown or pink end-point as described above.% s' [( F* A" M; i, v
Calculation:# p* ]. H5 X/ d$ y' Q( N1 b7 t
Calculate the percentage of aluminium oxide (Al2O3) in the sample
4 t: n" ?8 H+ ntaken by the formula:; _, l) W( ^; e8 W* a/ Q s' ^
% Al2O3 = 100 × (0.005VT)/S8 Z4 F w, k# w- ^/ f
where( t1 b' h, h# y. u( V: @5 v
V is the number of ml of 0.01 N zinc sulfate consumed in7 o8 T# ?; w' {6 T, ?
the second titration,) |1 ? u" W) [1 U/ G$ G5 X9 X
T is the titre of the zinc sulfate solution,
+ M' {! h" x' U4 u7 S5 d+ b0 H7 oS is the mass (g) of the sample taken, and
+ @% z- F: `4 h0.005 = 500 ml / (1000mg/g × 100 ml).
: T1 ?3 }1 t- b7 iSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica# e, \- P. y8 a# Q5 x3 b" q, R3 x1 ?
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
4 U5 _, n6 M m& U8 Q7 f! Q. rHeat gently over a Meeker burner, while swirling the flask, until
" T8 s9 I) H3 Y) D2 [ zdecomposition and fusion are complete and the melt is clear, except) S# l1 j5 B- o. N9 y p5 v
for the silica content, and then cool. (Caution: Do not overheat the7 C/ P% @3 ?2 f5 p7 k
contents of the flask at the beginning, and heat cautiously during6 u. N1 Z, c- p
fusion to avoid spattering.)+ b. ?7 I6 Z) B# u
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
. B5 y4 Q9 d# d6 W! s' dcarefully and slowly until the melt is dissolved. Cool, and carefully add
( ]6 |" I6 H* J: W150 ml of water by pouring very small portions down the sides of the. A+ j n9 }7 {; R8 m
flask, with frequent swirling to avoid over-heating and spattering. Allow
4 a& g S: _( H& a Z5 c8 w, X: ethe contents of the flask to cool, and filter through fine ashless filter
$ @+ P ?3 ^# n6 h* |paper, using a 60 degree gravity funnel. Rinse out all the silica from. _3 \; v u; i% u. B# ?& C
the flask onto the filter paper with sulfuric acid solution (1 in 10).
* |) l+ g! P& V* E; [. |3 }5 r6 ETransfer the filter paper and its contents into a platinum crucible, dry in
1 x% f6 t$ {/ z2 lan oven at 1200, and heat the partly covered crucible over a Bunsen
7 E9 S$ j9 c; w5 {5 F1 Oburner. To prevent flaming of the filter paper, first heat the cover from' D2 v5 g! X k" h+ J0 u
above, and then the crucible from below.
) j$ `# @! ]- s" d: h' T0 SWhen the filter paper is consumed, transfer the crucible to a muffle8 X0 l) X- z$ b, n1 @4 ?
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and/ z9 n" f$ _9 _' z
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
: T4 a: A( ~/ o8 F) ^' @hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first; c8 \, E, |7 L& b; i
on a low-heat hot plate (to remove the HF) and then over a Bunsen9 C2 q3 B6 X* p$ ^) S7 [$ e0 a
burner (to remove the H2SO4). Take precautions to avoid spattering,
+ F2 e( o& L1 c$ R! ~6 z/ E3 v& Eespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
. @: E1 E9 p' v; `# m1 s3 ]desiccator, and weigh again. Record the difference between the two
5 G4 G- |" [( |weights as the content of SiO2 in the sample.
( n( `6 `, j, M9 ^* PMETHOD OF ASSAY3 \' ]: F, E% v
Accurately weigh about 150 mg of the sample, previously dried at 105o
. O# Q9 e+ G3 t, K# Dfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
$ C* A! f& L8 Dand shake until a homogeneous, milky suspension is obtained. Add 30
6 [4 n# r2 z% D7 tml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
& X. x) z1 J3 ?/ F" H4 Theat gently, then heat strongly until a clear solution is obtained. Cool,
8 g+ [5 d9 ]2 d# `& D8 hthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric, [4 h% W) ?, R' w& b( C% D
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
7 P" L( H& M' r- @5 h2 _ g+ Arubber stopper fitted with a U-shaped glass tube while immersing the! |5 v* B! @7 m! d9 @
other end of the U-tube into a saturated solution of sodium9 i- w& ?* ? t) o3 b" E7 L
bicarbonate contained in a 500-ml wide-mouth bottle, and generate9 X. \9 j1 }# O6 c' e: ^! c0 [
hydrogen. Allow to stand for a few minutes after the aluminium metal
! P; F7 v8 n! Y; [has dissolved completely to produce a transparent purple solution./ y7 @$ e3 ]1 D
Cool to below 50o in running water, and remove the rubber stopper
L( W4 I& `8 {9 Z4 P9 U7 b0 M& Qcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
# v# g! b) f/ ^" Jsolution as an indicator, and immediately titrate with 0.2 N ferric
& Q5 E7 p" t5 s1 Xammonium sulfate until a faint brown colour that persists for 30
$ B8 e1 f8 T! t2 _seconds is obtained. Perform a blank determination and make any5 k3 J8 q% I: t6 K! a
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is) U# ~$ h- V E$ H0 w
equivalent to 7.990 mg of TiO2.' k5 d0 K& `8 c& e
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