|
沙发
楼主 |
发表于 2008-5-23 12:10:00
|
只看该作者
二氧化钛(钛白粉)
二氧化钛(钛白粉): ~- p1 i0 B( u4 a% v
) P6 d( c+ B* PJECFA关于二氧化钛(钛白粉)的结论1 T. ?$ d9 @! k$ m
* Z" \$ s* j$ g8 e
摘要: 2006年JECFA关于二氧化钛的结论3 \2 A! O# X: E \3 a+ u
ADI值:不作限制。+ J) K4 C8 E% N. i7 m& w8 q5 Z" G
功能:着色剂
9 u2 s$ A1 C1 ?. e+ U- G6 D6 `: i3 u9 u' ~% P
TITANIUM DIOXIDE
6 {) n3 k" |/ `Prepared at the 67th JECFA (2006) and published in FAO JECFA
|9 F0 n# y6 l" X- CMonographs 3 (2006), superseding specifications prepared at the 63rd
; ^: ^) A' |; G2 RJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
5 L+ a' r3 R7 Q' ?3 LCombined Compendium of Food Additive Specifications, FAO JECFA" J; M3 i; u% e
Monographs 1 (2005). An ADI “not limited” was established at the 13th
6 F2 W1 A9 E- W EJECFA (1969).$ @2 P/ _' n3 r( r0 g
SYNONYMS" P2 C; t5 Z" g. i3 d
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
u2 `+ o9 L9 x8 qDEFINITION
w- A( ? ]/ O9 I3 g8 |3 ]Titanium dioxide is produced by either the sulfate or the chloride* f/ P6 F& B3 L2 X" ?
process. Processing conditions determine the form (anatase or rutile
( E8 x: w5 p+ v/ |+ n" p% Jstructure) of the final product.& E, Z% K, J B$ I9 ~$ i$ [1 j* ?- U( {
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3), T1 L: O) W I! {4 x9 O% D
or ilmenite and titanium slag. After a series of purification steps, the, p, |' n- X: g7 b# v( r8 E
isolated titanium dioxide is finally washed with water, calcined, and% `/ D6 f. u' l
micronized.0 U+ e2 p' k2 ~( Y0 Y% W* i
In the chloride process, chlorine gas is reacted with a titaniumcontaining
5 M7 t- T0 S& R2 C- p6 Xmineral under reducing conditions to form anhydrous# L) t7 _# o0 x- \" K# g. m
titanium tetrachloride, which is subsequently purified and converted to% [3 j/ | f6 Z7 f
titanium dioxide either by direct thermal oxidation or by reaction with
, s* ~3 b; V) \6 G4 a# Y1 Xsteam in the vapour phase. Alternatively, concentrated hydrochloric
9 ` L) \ Y& E* aacid can be reacted with the titanium-containing mineral to form a2 x/ E# ^- \: y+ g- G6 Q8 g
solution of titanium tetrachloride, which is then further purified and
& @3 X) Q! G& {9 T( l" ^$ V+ uconverted to titanium dioxide by hydrolysis. The titanium dioxide is6 M& d* H9 q1 A, f7 b: p, H
filtered, washed, and calcined.
+ f1 N1 v" V! WCommercial titanium dioxide may be coated with small amounts of
& K' v) w, h/ b8 S3 W5 Ialumina and/or silica to improve the technological properties of the
; O" |- d8 j) ?" ]1 y- }+ J( Qproduct.
: e& W1 c& b9 YC.A.S. number 13463-67-77 f9 k) a2 }$ H* i2 T, n! a& D8 h$ k5 p) C
Chemical formula TiO2, F% ?2 o( Z( ]( T) P- `+ O! ?7 i3 Q
Formula weight
* s. I P' |0 o& Q" |79.88
% t: y0 ^1 [7 H# t" uAssay
" H5 H7 y0 Q$ ~( e( f1 L, w7 ]Not less than 99.0% on the dried basis (on an aluminium oxide and4 S, O6 i k6 U4 }7 k
silicon dioxide-free basis)
- D) `1 {4 ~+ y' C* fDESCRIPTION3 i9 x% F& y" H, t( M( p" b% ^
White to slightly coloured powder. G) r2 N" V0 J- q- t3 s p. L8 Q, H4 R2 a
FUNCTIONAL USES& a$ N( U6 I7 l- f$ B
Colour
2 g; F8 V& j' A5 n- ZCHARACTERISTICS5 Y$ r% |' u. \" e3 ?8 Q0 _3 R" [
IDENTIFICATION
( c8 \6 c* z$ zSolubility (Vol. 4)
/ [9 v2 p) p$ n# r8 r$ eInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
; X* f0 Z7 Z6 \/ zsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated2 }& i$ k7 ?1 ^
sulfuric acid.+ G6 V2 p7 X$ h1 }: _- }1 c8 }% L
Colour reaction
4 q9 L: G' r+ `Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of$ k4 X+ X+ S/ S8 S" y% \/ H: g
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
; [! Z9 s9 E" x/ F+ twater and filter. To 5 ml of this clear filtrate, add a few drops of1 c4 X7 ] s, c$ t
hydrogen peroxide; an orange-red colour appears immediately.! ~% Z4 e$ k5 n0 y
PURITY: B/ y4 ] J; c
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
: b# D0 b1 M5 M7 n1 FLoss on ignition (Vol. 4)# q6 O! `2 E( L; g' W% U, K( n: K
Not more than 1.0% (800o) on the dried basis
. ~" D y% h$ b. \3 }Aluminium oxide and/or3 }" D$ B3 U* V3 O6 [! m; J. {7 u
silicon dioxide
W9 g$ n$ j; W' F5 s3 x: mNot more than 2%, either singly or combined
/ F" @! m! b3 y' ~) bSee descriptions under TESTS
( }% B% P; u2 [5 U0 R- Y1 g; c7 xAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
) I# s( I* x* o4 @5 dalumina or silica.; W7 ^2 W; m0 U4 S, B$ I
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
- ^8 Z5 I8 l4 I% k7 jplace on a steam bath for 30 min with occasional stirring. Filter
( t7 x# ]6 m& W$ V: ~through a Gooch crucible fitted with a glass fibre filter paper. Wash. d$ r3 T3 @5 o- i \- d3 b9 L8 }' J
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
" o; Q2 J+ m* V- |/ D; Ucombined filtrate and washings to dryness, and ignite at a dull red
1 u* M7 s9 T: E' ?0 xheat to constant weight.4 n: |: ?" K: s9 @. A: L2 K3 M9 v
Water-soluble matter
: v% X: ]# u2 T7 X N! \: S& c(Vol. 4)5 A7 P$ b5 f. G+ P" B
Not more than 0.5%2 p- ]* Q9 d9 @3 p& w
Proceed as directed under acid-soluble substances (above), using2 h8 |3 y" R! L4 O" Y3 m- Q" l
water in place of 0.5 N hydrochloric acid.( S( D& E7 x/ c; e8 ^& ?4 O
Impurities soluble in 0.5 N9 f$ e$ t T3 n
hydrochloric acid
7 V9 ~' @9 u0 V: r0 e" g. sAntimony Not more than 2 mg/kg
' v7 q+ {7 a6 c/ SSee description under TESTS+ Z& {! j& I: d7 g
Arsenic Not more than 1 mg/kg( \& y$ y5 n% W. S1 @0 d
See description under TESTS$ ]6 `- l% e0 v- g
Cadmium Not more than 1 mg/kg H [5 D% R2 O- q( ^
See description under TESTS" w% ?# f z7 c; \+ d
Lead( N5 U' x! y0 S9 J
Not more than 10 mg/kg. t+ @9 I) @+ {3 S7 F0 I0 L3 P
See description under TESTS, p$ l& U6 z: e7 m
Mercury (Vol. 4) Not more than 1 mg/kg
' ?: P! _/ ], ]8 x4 ZDetermine using the cold vapour atomic absorption technique. Select a- H- M2 X" s. z/ x# f( V
sample size appropriate to the specified level8 t, j# ^7 s; Y% \8 G+ I3 d
TESTS, J) z0 v4 c. M) F! x1 ?
PURITY TESTS$ E& H1 O7 i7 v; G/ z" [# m, s
Impurities soluble in 0.5 N
( z% V( r( _! Uhydrochloric acid' ]5 h" ?& V2 q, I" a& r' j
Antimony, arsenic,! }) n6 e- ?) r$ }/ q! n# C
cadmium and lead
; L: p* D* a. W! u- N7 Z(Vol.4)8 E L) p5 }; U3 z
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
' o' ]- [# `( Ahydrochloric acid, cover with a watch glass, and heat to boiling on a
( Z& j! M) x) q( `- ` f( }: }hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml7 }$ L! B5 I6 Q* k
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved! C l c. b5 Q) \% O" T
material settles. Decant the supernatant extract through a Whatman
; L2 o! u p6 N( i' E; eNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
' L% H$ _7 L- F- i9 S" S/ ovolumetric flask and retaining as much as possible of the undissolved" F. [' n+ c( d" r+ i u \# p; h
material in the centrifuge bottle. Add 10 ml of hot water to the original+ A1 z2 g: N' i* b" r
beaker, washing off the watch glass with the water, and pour the
% Z: h! ]: q. g( H icontents into the centrifuge bottle. Form a slurry, using a glass stirring. U6 x1 z ~0 `$ n8 H1 E9 \/ |% K
rod, and centrifuge. Decant through the same filter paper, and collect* G# v4 G' Z; ` C6 {- \
the washings in the volumetric flask containing the initial extract.
8 m" U5 s4 x: j. fRepeat the entire washing process two more times. Finally, wash the; K& f7 X$ v; {# q
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
! O% ^: L; Q# s8 U( vto room temperature, dilute to volume with water, and mix.
4 \( ?/ z3 Y8 t7 C" ?8 M- @Determine antimony, cadmium, and lead using an AAS/ICP-AES) x& u9 v+ E" H* J3 F2 {; l
technique appropriate to the specified level. Determine arsenic using the
' w1 L+ G' b% r) t7 Y" l5 Y/ F \8 e" U5 c4 aICP-AES/AAS-hydride technique. Alternatively, determine arsenic using/ k/ ~! G$ ]$ B# c) W" h3 f* Z
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than- Q U0 A0 W6 X" q
1 g. The selection of sample size and method of sample preparation T8 R! [9 O; B- |( Z$ G! z. p& g6 A
may be based on the principles of the methods described in Volume 4.
$ I. ~; D+ ?0 w$ z3 Y% e- hAluminium oxide Reagents and sample solutions
. \7 q$ M! l( w4 M7 _0.01 N Zinc Sulfate
7 Y4 C" j$ P4 L. pDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to- `& U3 n6 v$ m4 `, N8 |2 M
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
; ?: w' P6 V5 Xof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
7 L, k9 e$ X, U6 J$ rconcentrated hydrochloric acid, heating gently to effect solution, then
' |: X3 I9 j P1 w: ^' @* ltransfer the solution into a 1000-ml volumetric flask, dilute to volume3 D5 [+ X( ], O$ l, v1 J) V) h* l
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
& d% ]7 H& O* l% z$ ^+ Jml Erlenmeyer flask containing 90 ml of water and 3 ml of
( u/ n- [$ P& v% P( Oconcentrated hydrochloric acid, add 1 drop of methyl orange TS and6 e9 E9 F5 r; y4 C
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,- }' t. R0 ]: W3 s9 Q. N1 F
dropwise, ammonia solution (1 in 5) until the colour is just completely% D% J1 n. l' ?$ D! J. M$ E1 W7 g# [; y
changed from red to orange-yellow. Then, add:
; I3 }9 a2 ]: R \2 |( n" I% w(a): 10 ml of ammonium acetate buffer solution (77 g of" @# ]0 X5 _. C, K: S
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
: P4 v3 E/ u1 R C- U3 q# D3 W1000 ml with water) and
6 l" Y* U; ]$ Q(b): 10 ml of diammonium hydrogen phosphate solution (150 g* X9 K: S3 e3 h5 n
of diammonium hydrogen phosphate in 700 ml of water,( g8 P( d6 z. L# R% v$ `
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,: b: h' B3 @* j) o" I
then dilute to 1000 ml with water).2 z6 D5 q: M9 _+ b/ B
Boil the solution for 5 min, cool it quickly to room temperature in a5 [, X0 S o' l- R! L/ W
stream of running water, add 3 drops of xylenol orange TS, and mix.* N( N# U, @) F, d$ G
Using the zinc sulfate solution as titrant, titrate the solution to the first
6 `2 E7 s b' n8 ?6 P0 byellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
$ R- D8 Q& ?) e4 X4 c* [. xThis titration should be performed quickly near the end-point by+ j1 x( j4 \5 B7 k3 ?* D& t
adding rapidly 0.2 ml increments of the titrant until the first colour
) w* G0 Z5 _% U) Q; Gchange occurs; although the colour will fade in 5-10 sec, it is the true5 ^" ^1 s. \3 P
end-point. Failure to observe the first colour change will result in an# l1 B# [; n* W* T- C3 W
incorrect titration. The fading end-point does not occur at the second: k2 ^6 S* n/ [3 k9 m" ? d* Y6 K
end-point.)# ?- x# v: Q2 ]2 o/ x5 k1 S
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
/ R) O+ l& V& M7 p! e7 H) hstream of running water. Titrate this solution, using the zinc sulfate$ {/ i: n7 f& n! b% s' _
solution as titrant, to the same fugitive yellow-brown or pink end-point
) q2 P' F% h+ d4 h8 ^" tas described above.
5 t3 C2 J) m4 \5 A& D, H% ZCalculate the titre T of zinc sulfate solution by the formula: N1 p5 T, n9 M0 W
T = 18.896 W / V t }. {6 {! t. x
where
" X# `5 x _ |T is the mass (mg) of Al2O3 per ml of zinc sulfate solution$ ?; a5 U3 I6 R& q% d5 j( J
W is the mass (g) of aluminium wire
6 f1 [# Q2 V6 t1 e7 D* o/ y g8 ~V is the ml of the zinc sulfate solution consumed in the, [ E1 o( x0 g9 |
second titration/ t6 [+ M4 T" o& H& N! {" B/ a0 b
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
! N& y, u/ `! ~! ]) A3 ~( G! {R is the ratio of the formula weight of aluminium oxide to5 R5 E& V! X; V9 p% {" `. f
that of elemental aluminium.
% p; F; l% \$ Y/ z5 J7 {Sample Solution A
2 o; w/ d4 g7 n" I4 b" lAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
. u5 p/ F- L2 L) r5 J- U( O1 `5 Mglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).$ v. {' ~" c' \; X; S
(Note: Do not use more sodium bisulfate than specified, as an excess
- |+ t" L& D( ]0 Vconcentration of salt will interfere with the EDTA titration later on in the
0 y) Q% O" R" ]) Hprocedure.) Begin heating the flask at low heat on a hot plate, and2 A, e% T8 E! X* w
then gradually raise the temperature until full heat is reached.
& }9 k4 D# l" z: \" i% Y% I0 q2 A(Caution: perform this procedure in a well ventilated area. ) When! u6 L6 n; [ Z+ J; {
spattering has stopped and light fumes of SO3 appear, heat in the full
. L" ?! ? A- o2 z1 i& g1 sflame of a Meeker burner, with the flask tilted so that the fusion of the. r) o i# R, E$ F
sample and sodium bisulfate is concentrated at one end of the flask.
, i- u9 J2 v& r. sSwirl constantly until the melt is clear (except for silica content), but
7 d; p. d0 A2 U0 F7 F4 D! qguard against prolonged heating to avoid precipitation of titanium% Z' u% p6 ^6 W1 T% o
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
7 }+ c" ]- Y: Nthe mass has dissolved and a clear solution results. Cool, and dilute to% {9 ~3 n1 i1 s, k$ }+ x
120 ml with water. Introduce a magnetic stir bar into the flask.
. [# ~ T) ~; j' I3 aSample Solution B7 F, [$ K3 i6 u6 V1 x0 y
Prepare 200 ml of an approximately 6.25 M solution of sodium
. K- K7 e/ }2 B$ nhydroxide. Add 65 ml of this solution to Sample Solution A, while, N; q2 p; W" ?1 \' ?
stirring with the magnetic stirrer; pour the remaining 135 ml of the
/ f5 C* h8 ~8 `2 Y( l( F% o3 U% u& F falkali solution into a 500-ml volumetric flask.( K6 E _6 y* O' t* {% t# O
Slowly, with constant stirring, add the sample mixture to the alkali/ ?; V% Z- z8 N+ H- ]
solution in the 500-ml volumetric flask; dilute to volume with water,
3 Q6 y$ t" w0 S6 C# b2 j3 ?1 cand mix. (Note: If the procedure is delayed at this point for more than' Y9 I& X5 ]: R+ w# T
2 hours, store the contents of the volumetric flask in a polyethylene
+ e# N1 u/ R; v# U' k9 Q" G& Obottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),9 {7 H- x: H {' f/ n
then filter the supernatant liquid through a very fine filter paper. Label
3 r/ j1 Z; m. ]; t, t5 vthe filtrate Sample Solution B.0 G( q$ Z* y( H$ }7 ]! `" h0 V
Sample Solution C
8 X- N3 L/ K5 m3 ^Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
- C7 A( C: y x% { T" K# t" s m$ P; ~8 ^flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
: p# W0 W" d! j& j( Q2 U- q2 x0 y1 dsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02! Z* s8 p, x' u& L+ U
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is& g$ Q N' W: ?+ q
known, calculate the optimum volume of EDTA solution to be added3 W9 [+ W/ Y2 ~7 [0 c
by the formula: (4 x % Al2O3) + 5.]
( ^) i# w% k6 P ?Add, dropwise, ammonia solution (1 in 5) until the colour is just* }; X9 k/ J( p1 u. t E
completely changed from red to orange-yellow. Then add10 ml each
7 p- O6 c8 U& f9 @; Xof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
$ G5 l/ h$ v$ eroom temperature in a stream of running water, add 3 drops of xylenol
" W; @8 @* z: h. r2 o. Morange TS, and mix. If the solution is purple, yellow-brown, or pink,
! j& V' t4 s# k1 wbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired0 B: ]- F0 Q, q3 U4 V5 y4 t
pH, a pink colour indicates that not enough of the EDTA solution has
% O& C1 o% D4 C- v# f6 M; wbeen added, in which case, discard the solution and repeat this: K- K2 v6 L* b9 t- S6 r9 w
procedure with another 100 ml of Sample Solution B, using 50 ml,
( r! M; _& B6 Q2 Mrather than 25 ml, of 0.02 M disodium EDTA., B* m! z" ^6 E, }- A# j5 `
Procedure* a. p. {8 X9 z3 Y0 U# s7 J
Using the standardized zinc sulfate solution as titrant, titrate Sample o; Z4 m9 z* Z, D0 y
Solution C to the first yellow-brown or pink end-point that persists for0 r/ A* P" F C5 e; P' b
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
% ?% d0 o H. @+ b7 etitration should require more than 8 ml of titrant, but for more accurate
3 [. o E% }9 \) Kwork a titration of 10-15 ml is desirable.
7 u7 ], p1 a# Q8 U; cAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5* U: f' E9 E0 r# }, U+ s
min, and cool in a stream of running water. Titrate this solution, using
& g+ G8 f4 d: A- M; Bthe standardized zinc sulfate solution as titrant, to the same fugitive$ J- r \1 f7 L& A( d1 k: B
yellow-brown or pink end-point as described above.! y3 o, z! {3 L& K* q3 D
Calculation:
: x$ @& |) _: o8 D; h, O: @Calculate the percentage of aluminium oxide (Al2O3) in the sample
9 ^8 r* |7 ]' C, n, T( staken by the formula:
- _! l& s; S" o i. R- e: ?% Al2O3 = 100 × (0.005VT)/S0 B' B0 f2 w5 w" H" @: `
where: q2 O( C% Z" |* P2 O
V is the number of ml of 0.01 N zinc sulfate consumed in4 V) E8 Y( I6 o/ o4 i
the second titration,, P- a2 a7 \) f0 n3 g
T is the titre of the zinc sulfate solution,, k" i& j7 K$ f* F7 n. V
S is the mass (g) of the sample taken, and
% ]7 J0 }& F4 u7 \3 o) { z0.005 = 500 ml / (1000mg/g × 100 ml).( [# d6 f7 E0 e% S" e
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
4 i9 J! Z1 ~3 [& v: u4 C2 T# cglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
# p1 m& X' _) w1 A- XHeat gently over a Meeker burner, while swirling the flask, until
$ }& b8 e% c4 t6 J' Ldecomposition and fusion are complete and the melt is clear, except% Y' q9 M1 O* J' T
for the silica content, and then cool. (Caution: Do not overheat the* C. z, u$ J+ {
contents of the flask at the beginning, and heat cautiously during
+ M4 u: f5 q! a. ^fusion to avoid spattering.)% U5 l* Q+ ^: b
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
8 { x4 q) ?( a9 S2 h- a' B i( t% ?carefully and slowly until the melt is dissolved. Cool, and carefully add2 t+ V' r$ @4 [# s9 g% A& ?$ ]
150 ml of water by pouring very small portions down the sides of the2 D1 J" @; T2 s7 b$ V8 F
flask, with frequent swirling to avoid over-heating and spattering. Allow+ O# F* t" X* |) ^' u
the contents of the flask to cool, and filter through fine ashless filter
2 d7 r1 K% P, opaper, using a 60 degree gravity funnel. Rinse out all the silica from; j6 K5 g: R# |! ~3 |9 f
the flask onto the filter paper with sulfuric acid solution (1 in 10).
/ R, o5 T) T: c1 J9 {0 A' N+ |Transfer the filter paper and its contents into a platinum crucible, dry in0 f9 v/ w5 m* H0 k" F. R
an oven at 1200, and heat the partly covered crucible over a Bunsen
) g# D+ W' W7 x2 zburner. To prevent flaming of the filter paper, first heat the cover from3 s8 i. ~) J4 c' W( Y K
above, and then the crucible from below.1 V# o- t5 f5 |4 O& b. _
When the filter paper is consumed, transfer the crucible to a muffle
& l! {, a9 G1 W2 U5 P7 `: Y4 ?furnace and ignite at 1000o for 30 min. Cool in a desiccator, and8 A& H. c* `$ `1 `0 ?. |5 b
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
/ e' F9 @" {- J. N+ J1 chydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first( N. K( h' U0 r5 D
on a low-heat hot plate (to remove the HF) and then over a Bunsen
3 w! B* `2 k& m" m* ?1 {( Wburner (to remove the H2SO4). Take precautions to avoid spattering,- U# U, j5 t5 Y
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
+ r3 W {! L+ E& Vdesiccator, and weigh again. Record the difference between the two
$ r1 F& v( R0 H7 `2 r: m: n4 qweights as the content of SiO2 in the sample.5 F- |# _9 `$ q# m- F
METHOD OF ASSAY3 ^2 t' b0 g0 \8 b0 e8 v- x
Accurately weigh about 150 mg of the sample, previously dried at 105o3 y9 c( b2 d9 M& T- _; D4 p
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water- K2 W9 r6 J; d2 q
and shake until a homogeneous, milky suspension is obtained. Add 30* O) r$ t) H. w: Z0 x+ D8 M
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially$ {4 Z% @7 ~% E5 \
heat gently, then heat strongly until a clear solution is obtained. Cool,; ?* ]: _* q4 \3 q8 I, t# S( A' C
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric3 X& k+ {5 \# c* k% @4 `
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
& A( E1 M% B6 @5 I: \rubber stopper fitted with a U-shaped glass tube while immersing the
: J: j5 l# P0 f! K G/ i8 R9 {other end of the U-tube into a saturated solution of sodium
& K& H4 g d% q/ X3 ubicarbonate contained in a 500-ml wide-mouth bottle, and generate
/ p, y4 a3 f3 v, c2 V9 [hydrogen. Allow to stand for a few minutes after the aluminium metal
7 s) |: V8 C% w2 K6 g* C/ z/ v. m# dhas dissolved completely to produce a transparent purple solution.% e4 I# N6 y. l1 |7 c
Cool to below 50o in running water, and remove the rubber stopper* P) s: s+ u; X+ L+ u& |: t, E9 L1 X
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
& Y$ j0 `; O$ lsolution as an indicator, and immediately titrate with 0.2 N ferric
9 E+ K0 K3 x% v: ~ammonium sulfate until a faint brown colour that persists for 30
, k* F' D" g9 p5 N/ d6 r8 _: _( Iseconds is obtained. Perform a blank determination and make any
: u$ x3 T" Y' C$ Znecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
/ w T. G# ~- n( h. _4 Y8 c, l7 c- z2 Zequivalent to 7.990 mg of TiO2.
$ t6 k% d& W6 ^. v2 H5 ? |
|