|
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)
7 ^: @7 [4 g: y5 a. p4 L. c7 O8 F0 Y$ p9 o& t
JECFA关于二氧化钛(钛白粉)的结论3 p0 m9 v! c7 x' q
5 _3 v; {2 f; t9 K: d摘要: 2006年JECFA关于二氧化钛的结论/ N' j0 `6 \/ _! O# @/ W; ^
ADI值:不作限制。
0 {. l3 |; I) d/ d5 E3 u( F功能:着色剂/ L2 U) ]1 y# O1 C
6 f5 g2 j* r1 ?7 U$ ~' F
TITANIUM DIOXIDE
- }' r' [* Z4 l0 t' q' i5 c' N) UPrepared at the 67th JECFA (2006) and published in FAO JECFA0 @! b* x8 o" ], |/ [$ F7 i( k
Monographs 3 (2006), superseding specifications prepared at the 63rd* m, v8 [% Z" K0 f4 j
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
( w( V. L$ i. {" m, e+ Y& Y' ]Combined Compendium of Food Additive Specifications, FAO JECFA7 u, Z! \/ }+ S
Monographs 1 (2005). An ADI “not limited” was established at the 13th4 r/ J# E% q) P+ R/ p# _8 L
JECFA (1969).
+ T8 N" h2 D3 @3 G3 WSYNONYMS7 y+ K' H, h6 v. N/ @% n3 \ l
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171# L( T: V) y( O
DEFINITION
: c8 I4 n) I( uTitanium dioxide is produced by either the sulfate or the chloride% V7 M5 n0 I, Q4 u( w
process. Processing conditions determine the form (anatase or rutile
5 U# X" A" ]" p) [structure) of the final product.
; k7 J) T) f8 l' @& d0 {In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)9 U. i! x* ^& W4 P6 \) E
or ilmenite and titanium slag. After a series of purification steps, the
2 X9 y2 h: U+ Z4 I7 e. q* oisolated titanium dioxide is finally washed with water, calcined, and
w' c6 u: h/ F' H% Hmicronized.
% m( F/ v5 i- gIn the chloride process, chlorine gas is reacted with a titaniumcontaining, S9 c( f" t) Y. K
mineral under reducing conditions to form anhydrous: C- ~) Y' ]& U
titanium tetrachloride, which is subsequently purified and converted to+ P5 v$ \1 o6 Y* I; `
titanium dioxide either by direct thermal oxidation or by reaction with
6 v: Y" U' n6 J$ s. s$ Psteam in the vapour phase. Alternatively, concentrated hydrochloric6 a! u5 Q% k4 k6 }* Q1 ?
acid can be reacted with the titanium-containing mineral to form a. r' \) J) [ B! Q
solution of titanium tetrachloride, which is then further purified and
$ x4 p. F: z4 ]4 B0 H2 v- Zconverted to titanium dioxide by hydrolysis. The titanium dioxide is' o# e% j6 v: n" ^9 U: v* ^
filtered, washed, and calcined.& s8 N; a# V$ m# t- e5 o
Commercial titanium dioxide may be coated with small amounts of
( _5 L: }$ K8 m, u7 Yalumina and/or silica to improve the technological properties of the( U9 d' I5 e+ H1 Q5 M
product.( Q; |* w& h$ c, J& r
C.A.S. number 13463-67-7
" B( \1 \ P- t+ N9 E" Z' c/ u5 YChemical formula TiO24 k5 L. U8 @" H% U
Formula weight0 a, z$ T) s, Y l
79.886 P. b! k f. [1 b+ O' W
Assay
4 `* K: ]' ^! l) ~Not less than 99.0% on the dried basis (on an aluminium oxide and
, L6 G$ R1 \- T- C w7 d( I" i3 osilicon dioxide-free basis)( b1 D7 F$ q1 z8 E( A9 g
DESCRIPTION8 s1 A1 N3 d3 X- g, x
White to slightly coloured powder$ c# Y' _; I; q& s. l; T& w2 q% h
FUNCTIONAL USES
2 N4 m! e3 G+ d8 B* G% RColour8 Z: w3 r2 i" N# r9 u2 b
CHARACTERISTICS
) j* O3 g8 G( D( E6 H3 ~4 a& g% E CIDENTIFICATION
: {# J* L, f# b# J6 o% ?Solubility (Vol. 4)
' ~. n8 N) n" `* @0 \0 _Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic5 c9 a7 t [4 P& E; d
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
+ ?9 f5 ?! f" s5 e Y; vsulfuric acid.
8 d/ b) E1 M0 C7 ]% z0 [ H0 rColour reaction
3 D3 ^% r' I% N3 |/ |; rAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
( I! g6 T* E B+ a0 k6 [( Fsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with" w* I* f9 E& @' H
water and filter. To 5 ml of this clear filtrate, add a few drops of
- v; k- m! x3 }2 P" ?1 qhydrogen peroxide; an orange-red colour appears immediately. K. ^- U2 `! A+ V: \+ q% U1 n! V0 h
PURITY
) r6 W+ n. h" o/ lLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)5 s2 T/ E# y2 D( C" s1 S2 K
Loss on ignition (Vol. 4)
9 M! x$ ] {% y/ f# m- D* x+ eNot more than 1.0% (800o) on the dried basis
5 y6 g j1 @1 FAluminium oxide and/or- Y0 C7 h+ N N5 h. a r1 g
silicon dioxide% J) N7 }$ n4 _3 D. U' D
Not more than 2%, either singly or combined
$ S. \# W* O8 y# g5 mSee descriptions under TESTS% w3 l) @) l2 u" ^& k. m" R6 T p8 r
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing2 N3 _2 z2 k$ U \+ M* w$ A5 l
alumina or silica.9 ^/ {# s8 T. z" j z5 l) j8 ]
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
4 x" k b$ s6 O& ?: |7 Qplace on a steam bath for 30 min with occasional stirring. Filter7 Q7 s6 I% K! X. o. o) w
through a Gooch crucible fitted with a glass fibre filter paper. Wash
, Z/ w; J: x! e) a8 ?with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
) g# X) N1 V. _: h7 E4 ccombined filtrate and washings to dryness, and ignite at a dull red" F8 F3 Y" ?7 v2 [3 O; ~5 t
heat to constant weight. [/ @ C! r( a7 F
Water-soluble matter
( k( y9 ~( g1 R( v+ ^(Vol. 4)
9 }' E1 n5 r A uNot more than 0.5%
7 x) u; s. p7 T% _" @$ CProceed as directed under acid-soluble substances (above), using
3 N- \7 t$ ?/ i5 v8 X! G8 j* qwater in place of 0.5 N hydrochloric acid.( s! @! E. O2 Y3 Q
Impurities soluble in 0.5 N
3 n2 C: { B/ ~hydrochloric acid
8 W8 l! b/ d9 s' S7 e- |, D+ _Antimony Not more than 2 mg/kg0 s# t7 \+ [6 N0 _ _" R7 r! x7 I
See description under TESTS0 ?. ~4 A8 |7 Q) i$ ]
Arsenic Not more than 1 mg/kg
; {# X8 V) o6 r4 J/ F. X7 z1 G2 lSee description under TESTS. j, u' O2 Q+ I( A4 {3 d& H3 Q M
Cadmium Not more than 1 mg/kg
, r# o& q6 ?$ P# s" v6 ~9 Y# ~/ ]$ i' H+ TSee description under TESTS
8 U: N+ O5 o8 ^% f2 @Lead0 H% o$ B z) ^2 @# i( ~* w
Not more than 10 mg/kg9 n$ S6 `5 C7 v" g$ k2 Q4 x
See description under TESTS
# P/ b! R( Q9 D& `Mercury (Vol. 4) Not more than 1 mg/kg2 ?$ m9 Z& J7 _% ?+ P
Determine using the cold vapour atomic absorption technique. Select a
) r: e3 H3 J' m! j0 X, z! Esample size appropriate to the specified level# r% W& G8 ~- _# p
TESTS
* Q" t3 x0 E/ d3 i5 `PURITY TESTS
. h4 N% `; h7 v, V2 aImpurities soluble in 0.5 N# ~6 J. c$ _* s' _+ R6 f0 K
hydrochloric acid
* L R! U/ ^0 g/ g# Z) O. HAntimony, arsenic,* b- j0 ]$ ?& c; h
cadmium and lead
B) Y! l1 K2 ?9 E% ](Vol.4)
- N; T* X9 K. z2 u4 tTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N* H4 q: @. k: V7 w- M9 e
hydrochloric acid, cover with a watch glass, and heat to boiling on a
! S' M* }; u6 n' ?- h" M* s, z2 whot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml7 d* s$ }. p, w- f" f! |
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
; w/ z: u7 I+ f% ?2 zmaterial settles. Decant the supernatant extract through a Whatman4 A/ m+ U5 I9 \% ^# }
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
* w* T2 W" w; P7 o* x1 Mvolumetric flask and retaining as much as possible of the undissolved% E3 ?8 n: t0 G- w- x) n& S& I
material in the centrifuge bottle. Add 10 ml of hot water to the original
: X2 D$ y6 ~" w2 x' u6 S8 Z. U ]beaker, washing off the watch glass with the water, and pour the3 [/ t) v3 O( z' k4 I& {; E
contents into the centrifuge bottle. Form a slurry, using a glass stirring
9 K% k$ }2 v7 p8 zrod, and centrifuge. Decant through the same filter paper, and collect9 @; M8 L7 _0 F( F( o9 Y
the washings in the volumetric flask containing the initial extract.
\3 t" |; F$ ]4 @; ?2 `+ GRepeat the entire washing process two more times. Finally, wash the
1 o" g# s5 Z# q6 Y* ?, O/ Y: {- xfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
7 A4 A6 Q3 o. z+ w( `to room temperature, dilute to volume with water, and mix.
0 h6 y* y% t& I+ [Determine antimony, cadmium, and lead using an AAS/ICP-AES3 Q9 h! o4 P \( S, e9 ~. h8 n) m
technique appropriate to the specified level. Determine arsenic using the
. j8 G7 O: U9 j1 ~& J: yICP-AES/AAS-hydride technique. Alternatively, determine arsenic using7 n$ Y" i8 Y1 c9 Z/ w: h
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than1 O/ ^) `7 t1 @( Y+ U8 S6 R
1 g. The selection of sample size and method of sample preparation
- M6 n% A# Z8 d6 |# H; Tmay be based on the principles of the methods described in Volume 4.
+ V# {! n8 i p( D6 ~' C7 PAluminium oxide Reagents and sample solutions
9 s0 v4 I9 j: ?) G0.01 N Zinc Sulfate* j8 f, C, O. t4 |
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
( B' G, j2 T" c" r l* H. \make 1000 ml. Standardize the solution as follows: Dissolve 500 mg6 S" p; {- M' e$ [, G
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
. X9 O3 H6 T. U! R% yconcentrated hydrochloric acid, heating gently to effect solution, then
" G" i' V3 z, z2 K- D n1 u$ Itransfer the solution into a 1000-ml volumetric flask, dilute to volume; p; B1 L: i7 {. V9 D; r
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500% @4 T- B) ?& J/ V9 G9 s4 Q5 U# l" I
ml Erlenmeyer flask containing 90 ml of water and 3 ml of& j4 I% V$ e6 q
concentrated hydrochloric acid, add 1 drop of methyl orange TS and& m. @7 @, ?" q* c' B
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,. h+ O, u) C" [
dropwise, ammonia solution (1 in 5) until the colour is just completely. f, P6 Q! v" ^5 j- e- \
changed from red to orange-yellow. Then, add:! K3 b, h" O9 i! @0 N
(a): 10 ml of ammonium acetate buffer solution (77 g of. d& b8 q" y# q8 M
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
1 a& G* C5 {. S1000 ml with water) and
* T4 a7 _- {6 R1 Y1 r(b): 10 ml of diammonium hydrogen phosphate solution (150 g
4 G: L/ F. f9 @6 aof diammonium hydrogen phosphate in 700 ml of water,' x% N7 ?5 L0 {% p. |6 A, C
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
/ [: k9 k4 ^" [! s% l+ qthen dilute to 1000 ml with water)." C6 v# G+ l, }
Boil the solution for 5 min, cool it quickly to room temperature in a% P, p* N/ H5 K
stream of running water, add 3 drops of xylenol orange TS, and mix.
: ]1 D6 c7 H+ [# S$ x, DUsing the zinc sulfate solution as titrant, titrate the solution to the first
+ W7 O; s3 o: U+ [7 i' Fyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
$ g' J* Q2 n# TThis titration should be performed quickly near the end-point by
: {2 U0 {0 d( _, }adding rapidly 0.2 ml increments of the titrant until the first colour0 M2 a8 C0 C; ~' W. p
change occurs; although the colour will fade in 5-10 sec, it is the true+ }" h4 r9 S! x: G: ] `
end-point. Failure to observe the first colour change will result in an+ }. l% s! V( J& e. ]* O% x0 K2 Y
incorrect titration. The fading end-point does not occur at the second- c( `* a. i/ T1 H* _
end-point.)
2 @" J. m' C1 d$ g ?Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
6 G% |+ C% X" Z- ?9 _4 k2 V# \- ystream of running water. Titrate this solution, using the zinc sulfate( u& ?. k/ s9 a% j' p, w
solution as titrant, to the same fugitive yellow-brown or pink end-point% i5 w" J8 S/ l ^0 Y
as described above.
) Y( \4 B4 H# YCalculate the titre T of zinc sulfate solution by the formula:) X9 D; O* w4 h' P. l I; J# @
T = 18.896 W / V
, j( }7 P3 N& t, lwhere
# B; l0 \7 m( U. _' h5 d; BT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
/ s3 F2 `9 Y4 i9 \W is the mass (g) of aluminium wire
- t( S2 J1 ^3 s% z* O! Z& pV is the ml of the zinc sulfate solution consumed in the' ^' q5 e$ Z+ i8 e8 J1 Y1 ~- [
second titration# h. d5 [4 k6 L: f3 e3 `
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and: U5 q: m& D* I+ H0 S# @1 q# w: ]. ?
R is the ratio of the formula weight of aluminium oxide to- c/ r. D; T7 Z5 f# U3 W
that of elemental aluminium.
$ y8 @8 O; q& f6 B& USample Solution A' A( p( v- v8 ^2 Y: D! \+ |
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica3 {" P3 S* h! W; K. V4 m
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).9 k* P; R3 G. [7 ]! o, _
(Note: Do not use more sodium bisulfate than specified, as an excess
6 P% C* Z* |5 ]- Zconcentration of salt will interfere with the EDTA titration later on in the4 L/ \9 s& B0 m d" {0 [( {) n, l
procedure.) Begin heating the flask at low heat on a hot plate, and4 ? z' ?+ P2 y/ p4 U$ I
then gradually raise the temperature until full heat is reached.& ]! y1 O- S' ~: U
(Caution: perform this procedure in a well ventilated area. ) When! Q1 _8 `% z" d
spattering has stopped and light fumes of SO3 appear, heat in the full; Z% _1 \" _+ F$ M( n; v; m) f
flame of a Meeker burner, with the flask tilted so that the fusion of the B7 H* `/ p- J! V d3 l3 Q) v
sample and sodium bisulfate is concentrated at one end of the flask.- Y2 c4 Y% |' R
Swirl constantly until the melt is clear (except for silica content), but
+ f/ p% |" H6 N5 A$ _1 G2 Yguard against prolonged heating to avoid precipitation of titanium
/ j, G% R3 u/ u/ Q5 cdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until% O) N: u, f! `. W% }! R3 L: ]
the mass has dissolved and a clear solution results. Cool, and dilute to
1 w2 y1 C! c6 m3 h g120 ml with water. Introduce a magnetic stir bar into the flask.# b9 y0 L! b1 _# T
Sample Solution B1 G" O: y9 y" B7 a9 b( ^$ ^
Prepare 200 ml of an approximately 6.25 M solution of sodium
3 H O& k/ r6 {0 H d7 zhydroxide. Add 65 ml of this solution to Sample Solution A, while
# j( U9 I+ c& J1 J3 w: d2 y: G9 zstirring with the magnetic stirrer; pour the remaining 135 ml of the( C9 p) G/ } J# X5 ?3 [: N
alkali solution into a 500-ml volumetric flask.
9 j. C; O6 M( c# U1 ySlowly, with constant stirring, add the sample mixture to the alkali
8 r, Z: S2 @! D: L, @4 s6 }. lsolution in the 500-ml volumetric flask; dilute to volume with water,: ^$ \; A# ^) o2 m- @& m- B' o9 h& C
and mix. (Note: If the procedure is delayed at this point for more than+ U4 b% P# N& S6 v5 g
2 hours, store the contents of the volumetric flask in a polyethylene% J+ e1 H6 Q5 |; [6 _: F
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
* {2 w. n* O7 K4 p1 Qthen filter the supernatant liquid through a very fine filter paper. Label
( J. G! h7 y4 _6 v& \( o6 X2 vthe filtrate Sample Solution B.
; F+ F( ^5 A4 N& a% J3 n" ?, L/ R! xSample Solution C! N/ ?; X3 ?/ e/ d6 E
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer- L% I+ S3 c! g. r( c8 z- l
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid: N1 R l/ a; W) v. [* |7 n
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
- s7 [2 U. C! R/ ^. FM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
& Y* L: o! n9 s; D' }8 q7 wknown, calculate the optimum volume of EDTA solution to be added4 h2 \( P0 Q( K
by the formula: (4 x % Al2O3) + 5.]( Q+ K# U( d9 e- o5 J' P
Add, dropwise, ammonia solution (1 in 5) until the colour is just
; N+ q% k4 O* ^& j" Zcompletely changed from red to orange-yellow. Then add10 ml each& T* P# A4 e: R' r" I' y
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
: w! \% j) D. C4 F" c! troom temperature in a stream of running water, add 3 drops of xylenol! {! T9 [& s' x* Z
orange TS, and mix. If the solution is purple, yellow-brown, or pink,5 p, s2 Y* K5 Q. \2 n0 f" i! \
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired* | ]: k- `$ e3 a
pH, a pink colour indicates that not enough of the EDTA solution has5 s' N+ D# B$ F/ m
been added, in which case, discard the solution and repeat this& o& e- b9 h& ]$ b
procedure with another 100 ml of Sample Solution B, using 50 ml,) M; w1 q) ]( w7 ~+ `# [. M( N
rather than 25 ml, of 0.02 M disodium EDTA., K2 R0 T9 I, Y
Procedure
/ e: y4 e* g+ Y$ e" T0 KUsing the standardized zinc sulfate solution as titrant, titrate Sample
3 {: J1 L- H S% JSolution C to the first yellow-brown or pink end-point that persists for
$ K" _; T, x1 p! F1 t/ a/ H: |: z5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first/ W( h8 D' d7 w4 `: Y
titration should require more than 8 ml of titrant, but for more accurate
8 a( A4 i" F+ x ]- R6 Y* N! [work a titration of 10-15 ml is desirable.# F7 [" `$ G/ S2 s3 ?+ K% u
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
* F- ]; I4 F S1 B" Dmin, and cool in a stream of running water. Titrate this solution, using
& K' ~) W ^& k% Jthe standardized zinc sulfate solution as titrant, to the same fugitive
# O" y6 k- W. m! J8 Y- u6 x0 D9 dyellow-brown or pink end-point as described above.$ o( q4 e" |; S3 X2 V/ Q6 B( |
Calculation:! w2 |5 g. @& W- x6 l, G; l [
Calculate the percentage of aluminium oxide (Al2O3) in the sample
* v: n! }3 x. H) Etaken by the formula:
& U) `( _! V8 e& e% Al2O3 = 100 × (0.005VT)/S4 @9 e# C, @% E& Z* G- h" d$ T
where3 D: W/ o: {/ O$ @
V is the number of ml of 0.01 N zinc sulfate consumed in
) w9 t: `, x, E/ E7 j3 B* @1 \) cthe second titration,/ _# l* a o7 q4 f; @/ L
T is the titre of the zinc sulfate solution,
& F5 `/ m) g# D# G. a) U {S is the mass (g) of the sample taken, and
: t. Y9 O. _8 A, ^6 j- P1 Y0.005 = 500 ml / (1000mg/g × 100 ml).5 D& b" R+ \4 @
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica( r" c) d+ q- w. c& Y
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O)./ \$ I% ~( H; `
Heat gently over a Meeker burner, while swirling the flask, until
, }% B0 R% L8 [5 b7 Q9 zdecomposition and fusion are complete and the melt is clear, except
6 k! J8 |4 s9 Afor the silica content, and then cool. (Caution: Do not overheat the( L- w0 B# w: k% R' k/ D
contents of the flask at the beginning, and heat cautiously during7 x! g7 d$ Z4 [; h
fusion to avoid spattering.)
# q% w" h5 |' K) t5 lTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
, Z* m2 `+ {" Ecarefully and slowly until the melt is dissolved. Cool, and carefully add
}( q. ~+ [7 b4 g. ^4 }5 |- C150 ml of water by pouring very small portions down the sides of the
# u7 t C9 f# M4 R$ L/ Y6 zflask, with frequent swirling to avoid over-heating and spattering. Allow* } O2 Z x+ S4 o3 m8 |" f, G# F
the contents of the flask to cool, and filter through fine ashless filter% u1 N' R: k3 I% z b2 X
paper, using a 60 degree gravity funnel. Rinse out all the silica from
+ v4 k7 U/ p! }& Uthe flask onto the filter paper with sulfuric acid solution (1 in 10)." A1 I1 F1 H; R$ z9 ~1 j$ B3 \- d
Transfer the filter paper and its contents into a platinum crucible, dry in
, k/ g3 m7 g; Zan oven at 1200, and heat the partly covered crucible over a Bunsen
( T7 V8 ]1 }2 c4 L6 ?burner. To prevent flaming of the filter paper, first heat the cover from
& \& v P3 B5 U+ Eabove, and then the crucible from below.8 b1 E* x" g9 D/ C: |+ O
When the filter paper is consumed, transfer the crucible to a muffle) g" F# m9 V f( H
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and' k- H6 B: c. C& Z# p# z; a+ y
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated8 N# y" k9 g9 T. U/ z" p5 u0 l! k
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
0 f( p7 V# Q n$ q0 Won a low-heat hot plate (to remove the HF) and then over a Bunsen
3 J+ e' V8 z7 ~- U5 Y. m. rburner (to remove the H2SO4). Take precautions to avoid spattering,7 {# N& q r0 Y( Z# K1 Z0 ]4 G
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a6 _/ _# u2 _- Y
desiccator, and weigh again. Record the difference between the two! F6 @, r' ]+ G! ~ `: D6 w( E
weights as the content of SiO2 in the sample.3 d- D2 g' R% C/ R6 F9 U4 C- {
METHOD OF ASSAY
/ P0 ?1 ?5 G5 `& b! |+ jAccurately weigh about 150 mg of the sample, previously dried at 105o9 c( V$ G$ n; ~5 W9 j& S! d
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water1 z3 A, ]1 E+ y9 u
and shake until a homogeneous, milky suspension is obtained. Add 30' k- B& }2 g4 G, u# {
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially ?0 Y2 h; Y4 M- b. S) u" U" ^" i
heat gently, then heat strongly until a clear solution is obtained. Cool,, k8 d$ m% y* n( N
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
% v& C9 M' R- q) ~* j ?+ Z7 }acid, and stir. Add 3 g of aluminium metal, and immediately insert a
2 a3 I" v) U- Nrubber stopper fitted with a U-shaped glass tube while immersing the
1 S' F" k3 x: A' W6 K8 c- rother end of the U-tube into a saturated solution of sodium, C" K" n2 u4 ~5 J S9 t' P
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
$ l% u' d' g' e9 Yhydrogen. Allow to stand for a few minutes after the aluminium metal+ N$ `, l3 b% l! D/ k5 P) m
has dissolved completely to produce a transparent purple solution.- t) D, N' o3 C$ F+ g, V$ d0 L
Cool to below 50o in running water, and remove the rubber stopper. Q8 b" u! D8 ~# s+ t; g, M/ p
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate: n4 I9 e- C' k
solution as an indicator, and immediately titrate with 0.2 N ferric
5 _( S) |6 `6 \! ~- nammonium sulfate until a faint brown colour that persists for 30/ h; N, f/ c7 U- t" K6 _# k: y
seconds is obtained. Perform a blank determination and make any+ j4 V5 U; d* G: r" d6 C
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is& t4 h. v/ n6 m' {* i0 `' z1 v; E# ~- F& X: C
equivalent to 7.990 mg of TiO2.4 C6 h) v, ?/ c" T! D* M/ s
|
|