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二氧化钛(钛白粉)
二氧化钛(钛白粉)
: ^; Y& D, O6 |- X- t( E" I9 u% W, U* ^" h# O
JECFA关于二氧化钛(钛白粉)的结论
0 _8 ?; B) |( d+ X, f; p" ]" v% R1 f6 Z; K m
摘要: 2006年JECFA关于二氧化钛的结论
7 @) a! C3 M' q& ?" S+ W; ^ADI值:不作限制。 g& r" r0 c3 f/ |- ^ j5 ]
功能:着色剂
8 q, F% W5 S1 _! o, _; Q5 |# x0 X, }- E- |6 k
TITANIUM DIOXIDE
$ T! R& x$ T9 B2 p; APrepared at the 67th JECFA (2006) and published in FAO JECFA* Q- L6 x8 F! K0 x: z7 H) L
Monographs 3 (2006), superseding specifications prepared at the 63rd
8 {4 @, m( C% X" ?JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
* a% G) e4 S$ R! [' p6 X& iCombined Compendium of Food Additive Specifications, FAO JECFA
- G9 c* u0 n2 D- ~Monographs 1 (2005). An ADI “not limited” was established at the 13th
/ z7 t! }; j b+ i V5 C- vJECFA (1969).
: h4 j2 q0 L3 e/ E# ySYNONYMS
! o3 J% F1 a5 Z( e. c i& h8 [Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171; E* O5 \# n1 U7 I3 m
DEFINITION5 V* r& \$ [2 p& W2 G: z
Titanium dioxide is produced by either the sulfate or the chloride
" I7 d) \" J4 D7 a9 B }+ Zprocess. Processing conditions determine the form (anatase or rutile: ~2 y% ?/ }/ }" j8 b. n5 I
structure) of the final product.# B3 W7 A, k' b: } w' ?
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
6 }7 N% d# ?$ U" Bor ilmenite and titanium slag. After a series of purification steps, the0 S1 K& ]4 M% r( i+ W2 w
isolated titanium dioxide is finally washed with water, calcined, and; t% o7 M( l$ c5 z4 w; @& d+ M6 T! T4 a
micronized.
E g. L+ h+ \# z- BIn the chloride process, chlorine gas is reacted with a titaniumcontaining4 o7 [/ K1 S7 q1 s6 Y) m4 S* v% b
mineral under reducing conditions to form anhydrous
+ l; j2 `7 c& c7 |& @0 M/ Gtitanium tetrachloride, which is subsequently purified and converted to
6 C5 u2 I, J4 f% [4 Ktitanium dioxide either by direct thermal oxidation or by reaction with5 _/ S' U" ?; `
steam in the vapour phase. Alternatively, concentrated hydrochloric6 Q* c* I8 Q6 l6 S8 f1 q3 I, G
acid can be reacted with the titanium-containing mineral to form a! Z% o4 W" L. d# C7 F b% c. M
solution of titanium tetrachloride, which is then further purified and- D: e3 S' u9 Z U: |. Q7 x2 S0 M
converted to titanium dioxide by hydrolysis. The titanium dioxide is
9 \: c# s; x2 ]filtered, washed, and calcined.
& E5 W4 C) p( E% ]0 H9 f: U8 dCommercial titanium dioxide may be coated with small amounts of% n6 t3 w( a+ e
alumina and/or silica to improve the technological properties of the
% h3 @2 }% z# P* x1 kproduct.
8 E" q' k" [2 `C.A.S. number 13463-67-7' [* Z! q0 `0 H/ K! C! W1 }" y
Chemical formula TiO27 y$ C0 g& h1 n( E1 N) O* {
Formula weight
* } G( A- V V. W, D* a79.88
5 u6 i* ^: M0 W; U- oAssay8 M( p: O1 d2 c7 |
Not less than 99.0% on the dried basis (on an aluminium oxide and
& z7 q, h# ]2 h' A( gsilicon dioxide-free basis)- Y. c) U0 R7 g. w
DESCRIPTION
, H' Q, D; z2 e0 sWhite to slightly coloured powder" R* l; {. X' v8 n7 j. A
FUNCTIONAL USES
, }& {# ?: @8 ]; OColour, H# A; Z% {) N
CHARACTERISTICS
+ }4 n& g: n3 C( j2 J0 ?IDENTIFICATION
. O. S, W( z6 s# MSolubility (Vol. 4)! u) F m, V/ h2 G
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic$ c; I/ r: S+ [* t
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated4 L8 Q, B M6 v4 v
sulfuric acid.
$ V0 w5 A. d7 O+ Z4 l5 k% kColour reaction
& ^9 \5 \) u3 z( P, R4 ?Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of, @7 E, x' S0 ~7 b' k+ F& C
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
4 v6 Y& T! M( Z% l7 Hwater and filter. To 5 ml of this clear filtrate, add a few drops of
" G, c8 r2 z* w' u1 x( Y/ J! j/ Phydrogen peroxide; an orange-red colour appears immediately.! i8 s4 ^5 Z. o& O. ^. C; `
PURITY6 Q0 H( {7 d5 R6 n8 R0 G% R4 l+ X
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
' W2 @7 K* U Q5 D/ _Loss on ignition (Vol. 4)4 _6 ?3 A3 h5 k
Not more than 1.0% (800o) on the dried basis
1 w* G0 f+ s# X( eAluminium oxide and/or
: I" `7 U$ r* L5 O/ b% g+ Fsilicon dioxide8 Q' @$ k+ ^$ R9 Y
Not more than 2%, either singly or combined3 j" ?8 L, z9 W0 f0 S5 @% b
See descriptions under TESTS
& |. c0 K9 H! y7 `9 j, GAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing8 O& K& S- h& z& R, d; ~
alumina or silica.
: D0 ^6 M3 f q8 nSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
/ F9 P, C4 }' C0 F, ?4 t% d. Iplace on a steam bath for 30 min with occasional stirring. Filter
, V6 @; K( y, m2 U T. vthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
+ d& H& ~% h. S8 _. k; uwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
9 a( n- t6 e" v: Ycombined filtrate and washings to dryness, and ignite at a dull red
+ Z; u& A a8 h U9 L5 T9 x4 aheat to constant weight.* N# w# W/ b& l, Q( t0 o
Water-soluble matter
$ b$ d! x! t$ H$ k' z7 G(Vol. 4)/ C9 y# G3 z. {/ ^
Not more than 0.5%
" J& I$ a0 X3 B: |; N9 C' Y# c9 ]Proceed as directed under acid-soluble substances (above), using
3 A& f! L% C' V! c' kwater in place of 0.5 N hydrochloric acid.+ I( O+ O) a) o. b
Impurities soluble in 0.5 N
* z! Y& R) g4 ^) q' x* @hydrochloric acid
6 |' o% l; w# O9 ?4 g2 a q, mAntimony Not more than 2 mg/kg
' t6 t5 X1 }# X& }3 kSee description under TESTS- }3 z9 W* e; y$ w3 f+ `3 m- K
Arsenic Not more than 1 mg/kg9 r4 E! k* I: O
See description under TESTS
" x" C8 U, Y2 k$ OCadmium Not more than 1 mg/kg6 U8 M, i3 p! c3 f
See description under TESTS; P0 G8 m' @& f3 ? d
Lead
: S# P: B( B. I7 U" ENot more than 10 mg/kg
c i- [( B1 H* K6 t+ D& LSee description under TESTS6 C3 f; ]. ?1 C- e8 E7 ?( x
Mercury (Vol. 4) Not more than 1 mg/kg A2 X" q1 N0 e3 i- h G. A
Determine using the cold vapour atomic absorption technique. Select a4 r4 {5 E+ f, T) P
sample size appropriate to the specified level
* q! [4 f7 a w0 Z @TESTS- u( c+ U5 s1 i3 C
PURITY TESTS& r0 Y. o8 X& Q" g$ [
Impurities soluble in 0.5 N4 Z# V" H, }, u
hydrochloric acid, j+ ]7 ~7 Y7 `, [/ v+ }, e/ p
Antimony, arsenic,: e& y* }! O8 e# Y$ f1 U8 t8 Z& r
cadmium and lead
8 }' w+ T1 N+ G, a9 \! u; B0 j9 f* C(Vol.4)
6 D$ |' K$ |- E/ L2 u4 g( E' N/ ZTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N" v' N1 ^" ?3 Y8 O3 @
hydrochloric acid, cover with a watch glass, and heat to boiling on a
3 S9 G. r7 c2 i. G5 \& O. H0 H8 Mhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml8 i7 f% q3 u' I `( O8 m1 c
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved, n, r* J+ C8 n+ S" O Z/ I& p5 S
material settles. Decant the supernatant extract through a Whatman1 ~# {: e1 C& ]$ T5 R. L
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
2 t( M3 y* x9 u* t9 T) h1 dvolumetric flask and retaining as much as possible of the undissolved' V2 C: i& `2 l
material in the centrifuge bottle. Add 10 ml of hot water to the original- }& L% y B% H( y- B: K& m
beaker, washing off the watch glass with the water, and pour the
. t# y, J9 g M" M5 l- `+ L: tcontents into the centrifuge bottle. Form a slurry, using a glass stirring
: L; a6 |; U5 k Mrod, and centrifuge. Decant through the same filter paper, and collect
5 Q, r: l7 I3 l0 L# |the washings in the volumetric flask containing the initial extract.
% u6 j9 _ S! D2 w( [% D6 L a0 ORepeat the entire washing process two more times. Finally, wash the
1 M7 c" G3 N8 p0 Wfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask/ Z6 r/ J# Y9 a! u7 H w4 }! c
to room temperature, dilute to volume with water, and mix.
+ G8 U+ ~% K- h& Y: }, q. yDetermine antimony, cadmium, and lead using an AAS/ICP-AES
# U/ \! v) D6 `% `: V2 Utechnique appropriate to the specified level. Determine arsenic using the
1 O- x" A6 w( x. x6 @* l7 HICP-AES/AAS-hydride technique. Alternatively, determine arsenic using+ |) L+ K! c' x/ C, u) ]
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than L0 u, L* x3 j& d0 }
1 g. The selection of sample size and method of sample preparation
1 K0 X) e2 W6 c5 J+ b7 Q4 Dmay be based on the principles of the methods described in Volume 4.# W2 H" f$ M6 _
Aluminium oxide Reagents and sample solutions8 x6 ?- I* n* t4 C+ n4 F
0.01 N Zinc Sulfate
$ |% i2 Y# u* F0 `4 }6 VDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
' G2 e: V8 d# i2 Pmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
5 h/ } h7 f J6 e4 oof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
9 R4 ` J/ N; ~6 h* [- I- Lconcentrated hydrochloric acid, heating gently to effect solution, then
$ U/ {% G/ P, n* Ntransfer the solution into a 1000-ml volumetric flask, dilute to volume
* X! ~2 H" O% _! Jwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
2 N1 X1 X, k* w4 ^0 a0 o3 ]ml Erlenmeyer flask containing 90 ml of water and 3 ml of
/ s- e; s- r1 f4 `concentrated hydrochloric acid, add 1 drop of methyl orange TS and
4 s& ?' [5 o7 }% A( d0 e6 a5 J25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
2 {; Q6 P9 }: { y4 C6 o5 d$ Jdropwise, ammonia solution (1 in 5) until the colour is just completely
/ q9 K* O9 b: v; |- O8 z0 schanged from red to orange-yellow. Then, add:; \$ h) n- K1 Y) a0 y/ c b
(a): 10 ml of ammonium acetate buffer solution (77 g of
$ E H! Z) A) a1 O& Oammonium acetate plus 10 ml of glacial acetic acid, dilute to5 e/ }* h8 d4 V# l9 s" g( w6 f3 M. i
1000 ml with water) and
E8 A& T$ v. F(b): 10 ml of diammonium hydrogen phosphate solution (150 g
% b% j8 V3 Y! R3 I1 j1 h3 zof diammonium hydrogen phosphate in 700 ml of water,4 |6 M3 K: j3 f3 H
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
. D6 d/ H* w2 w2 d* Athen dilute to 1000 ml with water).( C* z- E) i, s
Boil the solution for 5 min, cool it quickly to room temperature in a% p4 Y* W" n( k
stream of running water, add 3 drops of xylenol orange TS, and mix.
/ N! u: A% ~/ q1 I8 O! xUsing the zinc sulfate solution as titrant, titrate the solution to the first5 y6 m+ [/ x$ Y5 y9 [4 V& N+ N, `1 M! N
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
6 \: _/ [# g6 SThis titration should be performed quickly near the end-point by
3 V6 m# V F3 z* Jadding rapidly 0.2 ml increments of the titrant until the first colour
$ B# @' N& k6 z1 Gchange occurs; although the colour will fade in 5-10 sec, it is the true
5 r! X/ ?3 g7 _( @& mend-point. Failure to observe the first colour change will result in an
8 q) x1 E3 F5 m9 q' c m6 U/ D- Wincorrect titration. The fading end-point does not occur at the second. @+ {% j2 K- t' B# f9 k. U
end-point.)
; I T$ O; u" ~Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
( Z0 S7 C) i+ J+ kstream of running water. Titrate this solution, using the zinc sulfate8 n0 Z. z+ ]" V* h$ p
solution as titrant, to the same fugitive yellow-brown or pink end-point
W! ^2 D. [" v* P3 M7 O1 ^3 pas described above.
4 p% P& T$ R1 PCalculate the titre T of zinc sulfate solution by the formula:
% [* q7 t) K+ g( zT = 18.896 W / V! K) w6 J* G g# f' M; N, k
where
& Q$ z- u% M9 d0 ?0 gT is the mass (mg) of Al2O3 per ml of zinc sulfate solution# O5 J G* z7 c$ C* k8 b% O& G' m
W is the mass (g) of aluminium wire( \ D% \* ~2 i( h2 h4 d5 C
V is the ml of the zinc sulfate solution consumed in the
5 q+ f6 f+ O1 y8 f( b1 a/ @7 s" msecond titration2 F7 v! x, Y) X( E; `
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
& j% ?) ]2 n9 C; D0 w; M) O3 ER is the ratio of the formula weight of aluminium oxide to$ e) k- W, y" j2 b# x0 R
that of elemental aluminium.
/ r, a+ C9 F- r1 ^8 OSample Solution A
) V4 o$ h# l U* E$ }Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica) P) B% \ {4 I& |
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).7 d7 X. r+ x' T& P0 d X: f5 \) n
(Note: Do not use more sodium bisulfate than specified, as an excess
2 w- |2 b( z4 W- y5 d- Hconcentration of salt will interfere with the EDTA titration later on in the
( b: R& @& S: |procedure.) Begin heating the flask at low heat on a hot plate, and
2 O* V4 _$ I9 ]9 }4 ^* ], |then gradually raise the temperature until full heat is reached.7 n4 D" I0 w! y
(Caution: perform this procedure in a well ventilated area. ) When
6 d; n$ y1 m$ zspattering has stopped and light fumes of SO3 appear, heat in the full
9 Q1 t0 x: Q1 U9 j& |flame of a Meeker burner, with the flask tilted so that the fusion of the7 j! I6 k# Z- \: f } r5 a
sample and sodium bisulfate is concentrated at one end of the flask.
9 ~* i& x) w$ P7 K. d& x3 }8 jSwirl constantly until the melt is clear (except for silica content), but
6 u* A* q/ ?- J0 X- uguard against prolonged heating to avoid precipitation of titanium4 U; i0 B) _- l0 d T
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
6 D) ~# z# i, k% vthe mass has dissolved and a clear solution results. Cool, and dilute to- K, r- ?9 T) ?1 @: u3 a
120 ml with water. Introduce a magnetic stir bar into the flask.
1 S2 D; Q( D: @' k( GSample Solution B/ b( X0 L0 ^! j
Prepare 200 ml of an approximately 6.25 M solution of sodium% L" b+ ^: j; Q5 c
hydroxide. Add 65 ml of this solution to Sample Solution A, while: f" r3 z& E4 }# ~
stirring with the magnetic stirrer; pour the remaining 135 ml of the
$ S ^5 j5 L! Yalkali solution into a 500-ml volumetric flask.
/ F: d( s G! s9 HSlowly, with constant stirring, add the sample mixture to the alkali
. {$ w$ y& P$ q. a% R4 csolution in the 500-ml volumetric flask; dilute to volume with water,
. u* A. K6 y* Hand mix. (Note: If the procedure is delayed at this point for more than
6 p' N! D# R0 z4 A0 `2 hours, store the contents of the volumetric flask in a polyethylene# Y! o d3 I, M4 D) } {
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),5 X3 `9 C0 i, h
then filter the supernatant liquid through a very fine filter paper. Label1 F0 [& q* ~! s! p4 [# G" A& E
the filtrate Sample Solution B.9 s# Q, W! M, r. S
Sample Solution C
' V8 a( C& |2 [8 @; XTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer* |2 x& J) Z, h
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
* C) l8 u6 j ]3 Lsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.029 r/ B V3 N/ c; t6 K. o7 l7 f
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is8 V u* c, ^* B; Z |( b* u
known, calculate the optimum volume of EDTA solution to be added
9 U9 B- y* \3 a% K. t: Gby the formula: (4 x % Al2O3) + 5.]4 Y t! U0 j" d0 C
Add, dropwise, ammonia solution (1 in 5) until the colour is just
$ N4 | `8 F' r% N- qcompletely changed from red to orange-yellow. Then add10 ml each9 z* J5 i* k7 U% {, T/ w
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
9 A2 X, O% o/ |room temperature in a stream of running water, add 3 drops of xylenol! L, J9 T" q1 C! z) Q" u
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
/ m( a5 B8 v4 y7 U" tbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired( ^; R! n/ T+ I8 V
pH, a pink colour indicates that not enough of the EDTA solution has
7 d( s4 O# N$ f2 }& p% I& Hbeen added, in which case, discard the solution and repeat this
) I5 E# u+ e8 W# j7 uprocedure with another 100 ml of Sample Solution B, using 50 ml,0 X& L- F h4 z( f# w5 Z1 E
rather than 25 ml, of 0.02 M disodium EDTA.
. C; S$ \7 u1 ?4 pProcedure. ^: p- b4 ^( ^; Q
Using the standardized zinc sulfate solution as titrant, titrate Sample
9 V Q7 t& P8 u1 E! X% X& HSolution C to the first yellow-brown or pink end-point that persists for
2 }0 B* N" M0 Z) v7 i" ]4 @- {5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first; q; Y" x. `% [+ k# |9 I
titration should require more than 8 ml of titrant, but for more accurate) x( J" C5 a; w5 \, {) ]
work a titration of 10-15 ml is desirable.: ~, r' e& [- L1 N; U2 k# }
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5& ~" Y( C2 ]" g7 t6 ]6 `* W5 Y" ]
min, and cool in a stream of running water. Titrate this solution, using
: I# W3 c, d, K$ g5 J! A3 Cthe standardized zinc sulfate solution as titrant, to the same fugitive3 V" }& o+ l" Q3 `( Q2 S& j" m* \
yellow-brown or pink end-point as described above.
4 [" `$ x8 n+ _Calculation:
0 d. _! u6 M* P$ p8 {( CCalculate the percentage of aluminium oxide (Al2O3) in the sample; p) c& n; J$ w3 x5 o* n
taken by the formula:' O1 }2 l$ N$ z5 @' a R8 {+ H
% Al2O3 = 100 × (0.005VT)/S1 t( l) u$ a" F9 v* a
where5 P9 {' q- x. T$ ?. H$ J& P$ r, z
V is the number of ml of 0.01 N zinc sulfate consumed in
$ ~1 z1 `' n8 @* d! X7 w9 n Nthe second titration,3 N. t. |1 W0 n# r o' i( t
T is the titre of the zinc sulfate solution,: W! F% t* x/ ]1 Q: p' V/ M/ L. m( \
S is the mass (g) of the sample taken, and
6 o3 P3 |( c: R; O0.005 = 500 ml / (1000mg/g × 100 ml).' v/ {; @: o" n( l! W
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica' d2 L( N# W% A$ r" T
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
% j& r5 U4 ^2 a1 VHeat gently over a Meeker burner, while swirling the flask, until" p y9 H/ z5 r" h+ j9 i
decomposition and fusion are complete and the melt is clear, except$ V+ j7 Z& z% h2 j Q9 A
for the silica content, and then cool. (Caution: Do not overheat the
6 D6 u4 Y7 T+ \1 i2 i+ ccontents of the flask at the beginning, and heat cautiously during+ X. s! R. t: l- P! B" w
fusion to avoid spattering.)
6 F/ R) `* j2 Z5 pTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat* b: e$ e7 W/ f
carefully and slowly until the melt is dissolved. Cool, and carefully add# Y( F% ?! ^( I2 C6 T0 m; o
150 ml of water by pouring very small portions down the sides of the
6 P% K+ B! g) x1 I3 k0 `7 s$ lflask, with frequent swirling to avoid over-heating and spattering. Allow9 ?1 j% p( z9 n
the contents of the flask to cool, and filter through fine ashless filter
7 n( F6 m8 Z8 G3 ]paper, using a 60 degree gravity funnel. Rinse out all the silica from2 j D7 Z* d* j5 p
the flask onto the filter paper with sulfuric acid solution (1 in 10).1 {7 v3 c2 @, m" P4 u: B0 r; o
Transfer the filter paper and its contents into a platinum crucible, dry in
: J, L+ @/ R2 W. ~/ Gan oven at 1200, and heat the partly covered crucible over a Bunsen/ u2 b( j! z& g3 f% d5 a0 t
burner. To prevent flaming of the filter paper, first heat the cover from3 H& A; j3 U! i. e+ b
above, and then the crucible from below.% U5 \* e% r) \8 [) f$ w
When the filter paper is consumed, transfer the crucible to a muffle2 D$ ^: T/ [5 K% v
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and& Y3 c5 q& x8 R; ]
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
+ X. `3 S$ P3 X( ~1 ]hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first/ Z/ k" I. J+ |4 X/ s( Y$ O# j
on a low-heat hot plate (to remove the HF) and then over a Bunsen
' l& |- P2 R2 X4 a5 X& b3 aburner (to remove the H2SO4). Take precautions to avoid spattering,
# N9 a" l' Y5 ]- S, w& g; _6 n4 g4 Lespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a& v3 s" m" j8 V% ~6 C5 u1 Z
desiccator, and weigh again. Record the difference between the two
( w" e' n! n% A7 B, Vweights as the content of SiO2 in the sample.
9 `. [7 \/ U* c& ^# [4 JMETHOD OF ASSAY3 l7 R; c# D: G( G* |
Accurately weigh about 150 mg of the sample, previously dried at 105o: x- |* U- ^- j. S
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water# y( i0 `6 G* I7 K/ f5 A
and shake until a homogeneous, milky suspension is obtained. Add 308 T6 M& X6 {, }9 l& |+ ~# P
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially! u# \& ?+ }/ W9 r
heat gently, then heat strongly until a clear solution is obtained. Cool,
/ e n7 j9 U8 s% \" Uthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
" [. H) T$ I J# _acid, and stir. Add 3 g of aluminium metal, and immediately insert a
8 P# s E$ J+ _5 m! l, Arubber stopper fitted with a U-shaped glass tube while immersing the
, F8 a3 J% q l8 g/ N0 Uother end of the U-tube into a saturated solution of sodium
: J# ~8 @/ A& ~/ [% K3 fbicarbonate contained in a 500-ml wide-mouth bottle, and generate
% c+ |) ^- A6 A0 o4 _/ {: fhydrogen. Allow to stand for a few minutes after the aluminium metal
% }) Q8 b, G+ u" m& F; r' j; thas dissolved completely to produce a transparent purple solution.
& l9 W) p/ e: X6 mCool to below 50o in running water, and remove the rubber stopper+ o' x3 d- l! C) H' }/ y$ @
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
& R7 g8 i7 I; v# J$ b2 X( F4 i6 |solution as an indicator, and immediately titrate with 0.2 N ferric+ m& f/ a8 q; ~' e1 D: W
ammonium sulfate until a faint brown colour that persists for 30
( @+ u* |/ x$ k5 |0 Q1 {/ Pseconds is obtained. Perform a blank determination and make any) r7 _, E1 e; `: m
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
0 ^! J, {+ @8 h$ }) x3 Eequivalent to 7.990 mg of TiO2.
9 B. T8 B( q; I% V5 X |
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