|
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): K5 ^0 P, M8 ]9 A
% k, ]* D8 ~3 s* iJECFA关于二氧化钛(钛白粉)的结论
$ `9 C* X( M" N* e9 ~; i! }8 N9 S: j3 {, v3 x P9 [. A
摘要: 2006年JECFA关于二氧化钛的结论
, M8 g4 k; M* ^5 d0 q; xADI值:不作限制。
! U9 S$ B( F! J$ v d功能:着色剂
: Z2 C& W* s5 @2 y+ r
* \" S( K% w8 q" ?/ J; aTITANIUM DIOXIDE4 G- k2 k8 o) {7 J8 ?
Prepared at the 67th JECFA (2006) and published in FAO JECFA% C- Z4 ~, J. f( L
Monographs 3 (2006), superseding specifications prepared at the 63rd1 Z& ?6 d3 X' A5 I* {
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
( `% @( h2 G, ?8 c% UCombined Compendium of Food Additive Specifications, FAO JECFA
- Y; d% d/ O8 I& UMonographs 1 (2005). An ADI “not limited” was established at the 13th o& {; ?! F5 [# L! E: a) j
JECFA (1969).
1 M' N" N" l: O% l8 @& H1 W8 GSYNONYMS2 r: s. o& s4 Q3 v! a
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171$ C8 \: e2 I% s
DEFINITION
; U( |' t: g1 y* e; a0 H i) V; mTitanium dioxide is produced by either the sulfate or the chloride8 Y/ y$ K! f& ~" \$ j) A, L8 b
process. Processing conditions determine the form (anatase or rutile
9 {3 c9 }4 A5 l- Z; Wstructure) of the final product.
; _4 E# M# Y) D# ]1 p- [& rIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)% D2 a6 X4 y5 E/ ?1 F2 \8 [% q
or ilmenite and titanium slag. After a series of purification steps, the
0 M S3 U, q6 }7 Uisolated titanium dioxide is finally washed with water, calcined, and
) H% W5 {5 k0 v0 X4 n2 Umicronized.; e6 w2 s( H( E. ]
In the chloride process, chlorine gas is reacted with a titaniumcontaining+ r$ B$ m% ]! e9 y
mineral under reducing conditions to form anhydrous2 y8 j% p6 U4 K D; h2 C
titanium tetrachloride, which is subsequently purified and converted to
2 K3 N# q1 |% n2 ?$ A9 Q) utitanium dioxide either by direct thermal oxidation or by reaction with% A* j! [! x X# j+ I% R2 b
steam in the vapour phase. Alternatively, concentrated hydrochloric
" j+ C6 d/ o( G* D5 d3 P. uacid can be reacted with the titanium-containing mineral to form a
( H& H8 g B# Msolution of titanium tetrachloride, which is then further purified and1 f% d5 _# T. f" Z0 x0 z3 j
converted to titanium dioxide by hydrolysis. The titanium dioxide is
% J3 M# ?9 e* b/ a7 e) E) n- Ffiltered, washed, and calcined.! u- b; I( p1 G$ a/ ]
Commercial titanium dioxide may be coated with small amounts of T, }; H7 ?0 i( \0 T1 X7 L+ K4 L" W
alumina and/or silica to improve the technological properties of the' }- O! {- I+ x6 c6 O) g' Y" x
product.
& L9 X& r# E6 k. O* CC.A.S. number 13463-67-7& t7 l% l2 J/ X$ G4 d7 t; a9 b+ `
Chemical formula TiO28 V+ l* l: T# }& {8 k1 c4 u
Formula weight
; ~7 m1 [9 Z7 z, I79.88
1 J: p8 ~+ o6 ^$ a; M) ?Assay9 y& J' Z0 U8 Q6 c7 ~
Not less than 99.0% on the dried basis (on an aluminium oxide and' D% `3 a! p% \7 m7 S' Z5 B
silicon dioxide-free basis)
T. O- J& i' x+ h0 {6 q$ cDESCRIPTION& a+ B+ F7 O. r% r: R
White to slightly coloured powder
, W5 j, K% h8 R9 CFUNCTIONAL USES. b8 P" J, C; t/ n( F
Colour) `* O0 A3 O: j9 E
CHARACTERISTICS
! c7 V: E* J1 n) h( P ]IDENTIFICATION
3 `$ N- h' R0 a- V: hSolubility (Vol. 4)& R! I9 o) H7 l% J# n v( @& y8 a' g
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic) z4 \8 g. n6 o2 `3 J% v9 C+ D7 Z
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
* e9 V2 u: G/ Y. I+ Rsulfuric acid./ o4 i( K3 ?' l* d# }! A0 B1 H
Colour reaction$ Y2 ^: e& ~1 p! X" S3 R
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
7 [5 m9 Y. o: ~6 b4 u& v* B/ [sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with; [3 o& M* q# |$ P( R7 o
water and filter. To 5 ml of this clear filtrate, add a few drops of
' Y8 m+ T0 {( p1 f3 j9 \hydrogen peroxide; an orange-red colour appears immediately.
h2 [: b j1 {+ n! Z+ C4 ?PURITY( S/ y b$ {2 ]: C* J/ s% |
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
& M; ^6 T* t8 JLoss on ignition (Vol. 4)
; c4 m8 U3 r- X! X! S/ uNot more than 1.0% (800o) on the dried basis" l# T+ ?0 U9 ?# w
Aluminium oxide and/or% d6 M0 }( `- i; M
silicon dioxide8 V* m/ j- m, G5 p+ `
Not more than 2%, either singly or combined
: q+ t0 B4 F8 k% l8 y& X9 t/ aSee descriptions under TESTS
% j0 \8 g$ j, u% B" m, L8 i- BAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
6 Y- @2 n, J7 x) F5 U& ealumina or silica.
+ D ~0 v7 _5 `3 QSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and! C0 t, W" q2 \' y
place on a steam bath for 30 min with occasional stirring. Filter
% s/ u6 D! I$ G7 p/ b) A. Uthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
* [/ D6 l- d* v- A2 ^! A# ], wwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the- N6 o; x' Z. y: V% Z
combined filtrate and washings to dryness, and ignite at a dull red: u \3 G( }4 j: O
heat to constant weight.
0 K$ Z5 g' y( LWater-soluble matter
# F/ l5 W9 l1 R$ a" \' U(Vol. 4)
% j; f. I% b# o4 Y, K4 {Not more than 0.5%+ Y4 k: |8 {: l; x
Proceed as directed under acid-soluble substances (above), using5 t* x, F! m m+ o. _% c- Q! P
water in place of 0.5 N hydrochloric acid." e7 F& S' |+ I6 @
Impurities soluble in 0.5 N
( W3 x9 l7 C3 d% z2 zhydrochloric acid6 K( @/ f8 r2 ^
Antimony Not more than 2 mg/kg6 r, p8 H* K8 V! I
See description under TESTS
' H0 R5 F6 G' [' w; _7 NArsenic Not more than 1 mg/kg
/ y+ o0 z0 r( G, h: _8 }6 w oSee description under TESTS
; n' c% y+ t4 DCadmium Not more than 1 mg/kg3 [) R! I7 t Z
See description under TESTS: j5 T) i( e' D2 k7 R8 M( q& ^0 Q
Lead4 g& t) z7 `; O; p9 _
Not more than 10 mg/kg
& y8 f6 {3 {6 i) C- z lSee description under TESTS& Y/ V6 O# o& y4 r
Mercury (Vol. 4) Not more than 1 mg/kg2 D( H" B' E/ ~' E" i
Determine using the cold vapour atomic absorption technique. Select a
v. g: B- O ]; Z& f, K( jsample size appropriate to the specified level
v$ i/ |. B6 h! t GTESTS# Q& [! |( f! k. A% k4 i
PURITY TESTS
) a @9 Z* F+ e1 @2 r' r K' cImpurities soluble in 0.5 N
2 p" S1 F* r# [, Ahydrochloric acid/ ~7 s- Y `7 E2 ~2 D
Antimony, arsenic,* r' n# ~" S' M$ o7 a3 {1 ^
cadmium and lead% e# ~, e" Y$ E
(Vol.4): {' S# W. l: [& `6 A; ~
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N8 p% {' l9 Q" m) W9 [; |: N0 F- Q
hydrochloric acid, cover with a watch glass, and heat to boiling on a; v+ Q4 m: f, o. @4 G
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml8 {+ ]- n/ T! V1 d; _7 {
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved5 \8 ], x+ T- D2 z$ i: ^
material settles. Decant the supernatant extract through a Whatman
" o* ?* w; w+ VNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml, K/ p; l. A* N* g
volumetric flask and retaining as much as possible of the undissolved' Y7 ?, U2 h, l* x. k7 B$ R
material in the centrifuge bottle. Add 10 ml of hot water to the original8 N' E3 ~+ L# ^
beaker, washing off the watch glass with the water, and pour the
) @' W) L' h# T9 g0 J$ ^contents into the centrifuge bottle. Form a slurry, using a glass stirring+ n+ ]) Y8 R1 M/ k- i' ^
rod, and centrifuge. Decant through the same filter paper, and collect
4 L1 y' @+ A) Dthe washings in the volumetric flask containing the initial extract.
, ?3 j0 K# I: K: U) K4 }& y3 [1 ZRepeat the entire washing process two more times. Finally, wash the
4 N8 L3 X* H4 h. m4 ^filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
* e! X3 o1 {- L1 Nto room temperature, dilute to volume with water, and mix., B3 |$ O4 H& B
Determine antimony, cadmium, and lead using an AAS/ICP-AES( O3 R7 y" {6 M, l8 H$ y1 Y
technique appropriate to the specified level. Determine arsenic using the" V# i: G/ |1 e+ X2 g# T c
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using. Q# j( |1 x r) E4 C
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than/ L, Y: `. d$ ]! E, h- @2 e
1 g. The selection of sample size and method of sample preparation9 o( Q3 ]7 x( R8 w4 r& M: s
may be based on the principles of the methods described in Volume 4.9 n$ \6 R3 Y/ s5 c
Aluminium oxide Reagents and sample solutions
; I) o8 g/ |) N3 ^+ `, n+ w, d0.01 N Zinc Sulfate# U* z1 ~) L' j
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to6 ~" J! Z$ i) O' b
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
" p) l. v* T7 C# \ Cof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
( i. k% q! p5 H0 }: X' H. qconcentrated hydrochloric acid, heating gently to effect solution, then$ }# F* S( q% D% }8 h1 W- p( J+ O* k- }
transfer the solution into a 1000-ml volumetric flask, dilute to volume1 {& H( X: Z% ^$ G k( H. j' l
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500; {9 @3 O1 d& t: e6 F3 z" p* s
ml Erlenmeyer flask containing 90 ml of water and 3 ml of: a4 o# V- M) V* L! N0 s/ o+ \0 u
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
' N6 O% |" @' l' D25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,* }6 u4 Y2 o! H" L
dropwise, ammonia solution (1 in 5) until the colour is just completely
1 }7 _4 X9 \& P9 Wchanged from red to orange-yellow. Then, add:, f" q# M& m/ Z+ H8 I
(a): 10 ml of ammonium acetate buffer solution (77 g of9 p( C/ @1 }$ Q6 L* m9 m; {
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
9 l k% G2 M9 K X1000 ml with water) and
2 Z' G2 J9 E/ Y; }(b): 10 ml of diammonium hydrogen phosphate solution (150 g& Z) V. `8 _- T6 c2 U, i' Q5 i
of diammonium hydrogen phosphate in 700 ml of water,( S7 A) T" n3 m# P
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
+ `/ a7 n4 \& N" V) y2 n. ~2 C5 ?: cthen dilute to 1000 ml with water).
. ?, ^9 I9 e, o) K4 ~' _" h7 yBoil the solution for 5 min, cool it quickly to room temperature in a# j0 _; X, L" ^. ^" F8 @
stream of running water, add 3 drops of xylenol orange TS, and mix.9 _; z5 j, \) y! C5 w1 @ e
Using the zinc sulfate solution as titrant, titrate the solution to the first3 k U3 o0 A- d) _9 P( f
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:4 L0 ?3 N. M `' }, d L& A, {! D! s
This titration should be performed quickly near the end-point by
5 M- y. n. E+ d$ Zadding rapidly 0.2 ml increments of the titrant until the first colour
( I+ v$ P( p" H4 l& N6 l: qchange occurs; although the colour will fade in 5-10 sec, it is the true5 ~/ B* `& ]% v! j4 I
end-point. Failure to observe the first colour change will result in an
+ K& u% R" Z* ?- _7 }* R5 T& Nincorrect titration. The fading end-point does not occur at the second
* Q- b7 ~5 G# a- {/ F, M$ e. Tend-point.)
8 k& g/ ~3 a1 ^6 sAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a; c% N$ @& Z" _# d! Z# g
stream of running water. Titrate this solution, using the zinc sulfate0 b$ u" F4 b& ~* z, t2 j8 Q1 _
solution as titrant, to the same fugitive yellow-brown or pink end-point
0 i: s+ ]: t- H! g- U2 Q2 J9 Zas described above.
* d+ f; {) N4 v1 O) I( jCalculate the titre T of zinc sulfate solution by the formula:
2 T$ z0 d0 _) VT = 18.896 W / V# a v+ S: q- B6 C9 \5 U3 z
where) X, a# p) b8 v5 B
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
c7 {* C4 e1 G' w5 x0 ]! T* K0 rW is the mass (g) of aluminium wire' f4 J! ~" T& _* b
V is the ml of the zinc sulfate solution consumed in the- _8 }* O9 ]' t3 M! Q+ X8 q
second titration2 |5 ~ ^- P \
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and+ |/ Z4 R! I9 i
R is the ratio of the formula weight of aluminium oxide to; A+ \# q6 }! S2 E% k* W; z1 h i. {
that of elemental aluminium.
# F/ O2 X( p- T, Z7 kSample Solution A
& y0 U) w" L* QAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica; a; F) `) M/ i0 R
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
2 D* o% C" B7 T$ e. H1 t; g(Note: Do not use more sodium bisulfate than specified, as an excess
% W/ H! d4 C) X D. h3 s1 pconcentration of salt will interfere with the EDTA titration later on in the
# p( `; a2 j! P" S& y3 L1 ]0 Cprocedure.) Begin heating the flask at low heat on a hot plate, and# T! I* D, T! i" P" x
then gradually raise the temperature until full heat is reached.5 l- X L( M. \+ t# ]4 u
(Caution: perform this procedure in a well ventilated area. ) When# k! W- k# ?# [3 ^, t
spattering has stopped and light fumes of SO3 appear, heat in the full9 P! _# l% f! n* Y) J" X0 r8 q
flame of a Meeker burner, with the flask tilted so that the fusion of the4 h+ C7 Y. G" g
sample and sodium bisulfate is concentrated at one end of the flask.6 n. Q2 _; R# |1 l' ~ u) j. c
Swirl constantly until the melt is clear (except for silica content), but
: F" Q9 y1 E/ j7 S3 iguard against prolonged heating to avoid precipitation of titanium3 U' `% C. ]# O
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
5 ]$ x! |1 P+ j9 C( A6 q" fthe mass has dissolved and a clear solution results. Cool, and dilute to4 ]# R4 X& h' b) B! \$ f
120 ml with water. Introduce a magnetic stir bar into the flask.# B$ G2 j/ K1 c, Z Z/ V
Sample Solution B+ u R# }, N6 |5 O) Z) a7 f# Z( l
Prepare 200 ml of an approximately 6.25 M solution of sodium
; p! K0 O* @8 _; W2 Zhydroxide. Add 65 ml of this solution to Sample Solution A, while
4 ^% `! H3 k5 ^* \: _: Lstirring with the magnetic stirrer; pour the remaining 135 ml of the- A9 L/ Q" i! f1 y- W
alkali solution into a 500-ml volumetric flask.1 N7 I" n' X8 `. Q# A5 i
Slowly, with constant stirring, add the sample mixture to the alkali
4 f% R/ [/ k k% vsolution in the 500-ml volumetric flask; dilute to volume with water,
# X4 J0 L' ?4 ?6 @7 m. t" L* jand mix. (Note: If the procedure is delayed at this point for more than
- `& R4 F3 T$ \4 I: y+ F2 hours, store the contents of the volumetric flask in a polyethylene
1 C! r, r/ f6 E4 Ubottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),) B1 v T! }4 u
then filter the supernatant liquid through a very fine filter paper. Label! F0 I2 ] p9 O+ S: A8 I9 g+ G/ ?
the filtrate Sample Solution B." B @7 M; Y2 f- n" e" f
Sample Solution C
' m$ f4 V# m( c& jTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
! z) L3 W- e: e8 Jflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid* b9 r c) D! E5 ~
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
) K; S1 d" `# P* ?( C5 f' G6 }M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is% H* ]% ]( z- F4 G5 x4 ?) T* t: B9 {
known, calculate the optimum volume of EDTA solution to be added1 F! d& v( `7 l/ G
by the formula: (4 x % Al2O3) + 5.]4 L, W4 T: @! E) g: Y
Add, dropwise, ammonia solution (1 in 5) until the colour is just
8 G( w' ~2 K5 s$ M Icompletely changed from red to orange-yellow. Then add10 ml each# ]4 p3 V8 F( @( z" W9 _! y
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to! a/ @7 p/ c) r; |! J
room temperature in a stream of running water, add 3 drops of xylenol }1 B; l6 b6 X( S7 l( Z; j* t
orange TS, and mix. If the solution is purple, yellow-brown, or pink,+ `6 f( ~& {! a3 \
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired! ], o1 t" f s0 o# |& m
pH, a pink colour indicates that not enough of the EDTA solution has3 [0 Z* o7 J3 d( l- V8 b) B% @
been added, in which case, discard the solution and repeat this
" C1 V6 u/ [6 K, }# |procedure with another 100 ml of Sample Solution B, using 50 ml,) C( K/ _5 E6 O
rather than 25 ml, of 0.02 M disodium EDTA.
4 k& i) Y& O4 N5 c* C% BProcedure
5 D) K4 r/ C6 P# `6 t! lUsing the standardized zinc sulfate solution as titrant, titrate Sample
/ _: F" w) A2 ~4 X. u4 U9 fSolution C to the first yellow-brown or pink end-point that persists for
7 d7 Y1 ?* _* I& L4 L4 s5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
* O+ l3 j5 y: n) S! O' \8 z3 Ztitration should require more than 8 ml of titrant, but for more accurate
) b* z) X, Q; i' b) G! M) kwork a titration of 10-15 ml is desirable.) N* }, f1 d4 e' B8 W8 F1 q
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5( i. g6 m1 P$ ?8 H4 J, J* m
min, and cool in a stream of running water. Titrate this solution, using, }7 S! h( _: x" _
the standardized zinc sulfate solution as titrant, to the same fugitive
$ S8 ?, H8 c( a0 G$ a" j/ Iyellow-brown or pink end-point as described above.
7 R, n5 z$ l) f# a$ A1 A" O R/ eCalculation:$ B* ^' _# x Q# }+ s9 O, c6 h
Calculate the percentage of aluminium oxide (Al2O3) in the sample
' I( ^3 M- ], R# z1 etaken by the formula:
" `8 C' _# U) i9 ~% Al2O3 = 100 × (0.005VT)/S' Y0 I; M) g8 \
where+ J& l$ u' T( |4 e( k4 ?: F; Q1 n
V is the number of ml of 0.01 N zinc sulfate consumed in, l" r' \- \* ^# t- F" [# X& q0 \
the second titration,$ C1 V7 g2 b5 X+ y0 F
T is the titre of the zinc sulfate solution,
, S6 G; X! f* `! ^! @! z! A# j2 JS is the mass (g) of the sample taken, and
5 \# ]1 @5 B" |' V3 y0.005 = 500 ml / (1000mg/g × 100 ml)." I" O: a+ I" u( S0 H" f( P, _
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
5 t0 q& S) Y2 I9 S% t2 j# z) ?glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
3 P& \6 ]/ O1 gHeat gently over a Meeker burner, while swirling the flask, until
" \+ @2 V: `# C. n }$ Gdecomposition and fusion are complete and the melt is clear, except
3 j* ^ J/ p' p. x7 C; f% ?for the silica content, and then cool. (Caution: Do not overheat the
4 A0 P& M8 K; j6 R1 C: L/ B; [8 ^contents of the flask at the beginning, and heat cautiously during
4 R) u$ [/ M3 Y. C: `: }fusion to avoid spattering.)+ v, c6 ?" {2 `' W4 u2 |; W
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
8 P& x, k! z3 p7 D6 jcarefully and slowly until the melt is dissolved. Cool, and carefully add
3 M* [8 Y! ~0 N% C150 ml of water by pouring very small portions down the sides of the/ i6 N* e9 C/ b; L
flask, with frequent swirling to avoid over-heating and spattering. Allow9 L2 }% |/ ]/ k- m5 i
the contents of the flask to cool, and filter through fine ashless filter) D# l( R% e9 Y" f- X
paper, using a 60 degree gravity funnel. Rinse out all the silica from
+ m; [9 q- ]1 s( y: pthe flask onto the filter paper with sulfuric acid solution (1 in 10).
% j2 W" D+ y; \/ r# B$ t4 w1 QTransfer the filter paper and its contents into a platinum crucible, dry in
# U: Y5 a$ K4 x* Aan oven at 1200, and heat the partly covered crucible over a Bunsen
$ N* \( ]# I1 R0 P! dburner. To prevent flaming of the filter paper, first heat the cover from1 ^, r: d, v: y) f, F
above, and then the crucible from below.
$ O1 t9 ^0 R1 r; S1 HWhen the filter paper is consumed, transfer the crucible to a muffle: J& C# X9 q& b
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
7 P5 h2 i6 ?3 _; @( Fweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated- ^9 n3 {% G7 \1 N f$ X+ O% J/ b- @/ T
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
( e7 c/ G: [0 b/ T5 n' con a low-heat hot plate (to remove the HF) and then over a Bunsen
2 ~" v5 h& q5 T- Y; A) X- l4 ^burner (to remove the H2SO4). Take precautions to avoid spattering,% ]1 @ Y( [# U4 ?
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
! C" L( U5 K/ f8 x9 n! b/ m) ]4 _desiccator, and weigh again. Record the difference between the two4 k+ g% }! ~) v; m; F
weights as the content of SiO2 in the sample.
) X9 P" |" F r, EMETHOD OF ASSAY
3 F5 c$ _; ^8 N0 a, r2 e4 W9 qAccurately weigh about 150 mg of the sample, previously dried at 105o
: U3 Z+ J( m- Z2 wfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
1 ~" z M& |, |& mand shake until a homogeneous, milky suspension is obtained. Add 30
0 h0 C: k% U* u. M1 }+ _9 @ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
/ k) n# O7 `5 E/ W7 hheat gently, then heat strongly until a clear solution is obtained. Cool,2 q8 H& p; t) B
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric8 V* h/ z% F/ s- F; o
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
S0 P0 Y' H# U! _9 ]3 I" y5 nrubber stopper fitted with a U-shaped glass tube while immersing the
. @8 U7 U7 }& B5 O kother end of the U-tube into a saturated solution of sodium& H( {! G; f3 H( Y
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
1 a, O) K1 h% t7 ^hydrogen. Allow to stand for a few minutes after the aluminium metal
2 d6 P0 _+ O! X+ ?- Ohas dissolved completely to produce a transparent purple solution.$ j) K N% u/ Y) s
Cool to below 50o in running water, and remove the rubber stopper
( I4 t% C) z+ x% j7 b. x$ C. [carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
- U9 W1 C- w$ m, zsolution as an indicator, and immediately titrate with 0.2 N ferric& }8 T, y+ V1 P+ x
ammonium sulfate until a faint brown colour that persists for 304 {0 y% n3 H J! V. V
seconds is obtained. Perform a blank determination and make any
* d, o5 H, ^; ^% b( [" R6 B4 ?necessary correction. Each ml of 0.2 N ferric ammonium sulfate is* r9 j5 ~! n$ p
equivalent to 7.990 mg of TiO2.8 U# T, ]4 Z5 M: ` w9 \
|
|