|
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); n4 X9 T% [) H- M
9 i! c0 h. t2 `7 d, Z. F% u IJECFA关于二氧化钛(钛白粉)的结论5 \" n8 y `( V/ w; ~7 }: l
8 F) O: a, Q0 u* k/ r3 m! p: |摘要: 2006年JECFA关于二氧化钛的结论
& J4 `0 n+ v% t/ sADI值:不作限制。
t/ ]( N4 Z( i4 Z功能:着色剂6 N0 m2 H5 V; D8 D, x8 r8 V
* V2 R. r3 n( {, VTITANIUM DIOXIDE
* z7 [3 @1 E# c6 a) YPrepared at the 67th JECFA (2006) and published in FAO JECFA
9 u+ L/ m1 F: T1 E7 MMonographs 3 (2006), superseding specifications prepared at the 63rd
: v: s# o& V, ^) l9 jJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
7 \! R& V# L5 E. vCombined Compendium of Food Additive Specifications, FAO JECFA& m, H. P3 F5 S+ t( O
Monographs 1 (2005). An ADI “not limited” was established at the 13th0 E) `5 B7 p* B3 H
JECFA (1969).; c+ m; Y7 ^% m6 v% ?. ` |7 O+ T+ z7 k" a
SYNONYMS7 H" X. K1 h. F* f. m" e
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
' P4 y4 q4 v \/ [! {, ]* [0 UDEFINITION3 K: `" M; V$ s
Titanium dioxide is produced by either the sulfate or the chloride) N9 C6 F5 m, O( U& J
process. Processing conditions determine the form (anatase or rutile
1 u; s- `' b# b" bstructure) of the final product.. Q' O X% Q1 b) O0 c* y6 }' B* k
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
) R) e0 B& w$ Q0 L1 }or ilmenite and titanium slag. After a series of purification steps, the) a! L' t0 Y2 b: m, }" c( b, A: _! w
isolated titanium dioxide is finally washed with water, calcined, and
, O! f: F+ {$ n& [( u; g0 c, Rmicronized.6 i% M1 X0 v8 A( J5 n# ?" X0 F) `
In the chloride process, chlorine gas is reacted with a titaniumcontaining5 J" c, g* F! u8 t
mineral under reducing conditions to form anhydrous
- _) ^. p5 P, T8 v4 P Ftitanium tetrachloride, which is subsequently purified and converted to. \3 j/ |+ q) A$ o' r
titanium dioxide either by direct thermal oxidation or by reaction with+ Y( ]" m& }3 t* R3 F
steam in the vapour phase. Alternatively, concentrated hydrochloric# G! t# z% s' G
acid can be reacted with the titanium-containing mineral to form a5 G1 } J) f; E5 f; n
solution of titanium tetrachloride, which is then further purified and* R* |, e% s: R$ {
converted to titanium dioxide by hydrolysis. The titanium dioxide is
C- J3 z! F0 I7 Tfiltered, washed, and calcined./ y0 h$ ^+ _2 }: S0 O) o0 o
Commercial titanium dioxide may be coated with small amounts of2 n' F* G! y# n0 D
alumina and/or silica to improve the technological properties of the1 v9 n* O, v+ L9 S! E7 Z
product.; O. M& W3 R+ f0 X; M" k
C.A.S. number 13463-67-7
! ]% @8 ?: ]' VChemical formula TiO2; `4 Z6 j# R! ~; S: r# X6 E0 t
Formula weight9 L H/ C8 n. q/ l5 `; {3 W
79.88) W/ ~. f9 _7 Y5 d
Assay" U5 w2 f+ J/ n( F" E) q
Not less than 99.0% on the dried basis (on an aluminium oxide and1 v( h8 l& I7 s% x4 {# _7 K
silicon dioxide-free basis)
; M0 N) _! Y- N6 h* JDESCRIPTION
4 \* K- s, d5 PWhite to slightly coloured powder. e# t% C3 i" X& ]. y5 @
FUNCTIONAL USES
7 S! e" C& P+ J7 ]Colour
, g/ i1 ?! Z2 y5 Y: ^! RCHARACTERISTICS
+ L/ h+ s" Z1 l3 r) H6 UIDENTIFICATION
9 ~% j. g# y/ S. A5 G# NSolubility (Vol. 4)
% F) [1 i! q) \4 G. ]6 l) c# j8 [Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic$ ^- L" B3 J# o- n; h/ ]
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
}1 B9 m- B6 z4 [, c: esulfuric acid.2 V! _9 D {5 s+ v* ~
Colour reaction
/ c- B# Z1 _8 V2 A) a9 j9 wAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of T5 D; e. o1 f4 M$ I
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with/ w8 I+ G. v5 b
water and filter. To 5 ml of this clear filtrate, add a few drops of
( |$ j( B+ U/ l/ @( |hydrogen peroxide; an orange-red colour appears immediately.* ?) y: B( m3 b9 `. w: M. o
PURITY
. _ Z- i9 G3 o7 qLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
8 L+ X& Q( ^& V- l8 KLoss on ignition (Vol. 4)8 |7 ^1 ~! O# [! O! }
Not more than 1.0% (800o) on the dried basis; F* B3 N4 G! H3 ^) P
Aluminium oxide and/or) E3 ] i0 ~$ G; P8 ^* O3 _) s
silicon dioxide. k( z) J6 o- w3 H! p0 |
Not more than 2%, either singly or combined" Y% F h0 c/ A" U
See descriptions under TESTS& `- o4 G) ^- n2 j+ l- q
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing) P% k' P4 f6 V' d {3 l
alumina or silica.
7 N# I: x8 O( tSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and8 s" e5 c+ Z/ e. G/ i n
place on a steam bath for 30 min with occasional stirring. Filter
) d0 S$ ?" d0 `, @# K! Z" rthrough a Gooch crucible fitted with a glass fibre filter paper. Wash& u! Y: E2 s* U/ a
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
& D u7 h; r! s. Y7 \9 vcombined filtrate and washings to dryness, and ignite at a dull red
; E# e( X+ S. v/ u Theat to constant weight.9 w0 _0 {( d8 z; ?: ?3 W
Water-soluble matter
! G' v9 f$ h# {. D) h E/ Y: |(Vol. 4)
' G) p. H$ M& l( u( e5 BNot more than 0.5%6 G6 X" p* J* F: K# `7 T
Proceed as directed under acid-soluble substances (above), using
: c/ r. F6 Z# E0 K* r& V4 ?, O9 @water in place of 0.5 N hydrochloric acid.
. O9 @0 Y6 P3 a0 M, C& {2 SImpurities soluble in 0.5 N3 k; E3 Q, _( |# d: w4 j
hydrochloric acid
( o/ R$ @6 I# D% gAntimony Not more than 2 mg/kg
- R8 b& g" Q& ?! M. KSee description under TESTS& S/ S9 j/ ~0 b5 T" a
Arsenic Not more than 1 mg/kg
0 Y* d0 V1 Q- r+ v0 \See description under TESTS% T) {9 s/ z" x( X- u& Y, j! L
Cadmium Not more than 1 mg/kg
9 o7 d1 Q% A/ |( w1 ^: E2 _See description under TESTS% O6 S3 T) V% y8 J2 j
Lead! @4 F; v4 d# p& J: D8 j
Not more than 10 mg/kg
?' \6 R, A3 k5 eSee description under TESTS
; o2 ?7 Y! ^: e, i' L7 [8 CMercury (Vol. 4) Not more than 1 mg/kg( H: u0 F) }. w' a; i1 ]+ L) S! N
Determine using the cold vapour atomic absorption technique. Select a+ a1 \2 _ P& }4 ?7 A( g
sample size appropriate to the specified level
1 d4 c5 y: [1 G) dTESTS r6 X1 j/ h9 ~# @8 K: r- [9 L
PURITY TESTS
3 \, p$ J0 d* P5 gImpurities soluble in 0.5 N$ ^; I( }- T: |8 l5 ~$ _, Z/ [
hydrochloric acid5 Q7 R$ _& x1 n. X, O A7 m
Antimony, arsenic,
: P6 \) q$ B ?5 D# |; j H' M7 `2 |cadmium and lead
1 G1 r" _, S) \(Vol.4)
2 I0 ]6 L) n4 Y l: `Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
3 m& q# C* v( X" G8 thydrochloric acid, cover with a watch glass, and heat to boiling on a/ |7 h" t4 q+ N% ]$ i
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
7 [* h4 t6 M }( ]$ m( {centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
& K) Q8 l6 U8 P8 b- L0 hmaterial settles. Decant the supernatant extract through a Whatman
* F) O' O; }4 M8 x% T, vNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
7 l" V( [0 N9 F& A. v/ h# Pvolumetric flask and retaining as much as possible of the undissolved
5 l( {" y! s5 B) _material in the centrifuge bottle. Add 10 ml of hot water to the original
8 b- S- o7 _9 N7 h; rbeaker, washing off the watch glass with the water, and pour the
V9 J( r& `0 q& C4 S* pcontents into the centrifuge bottle. Form a slurry, using a glass stirring
5 R2 @ h, o$ _' g( |* @rod, and centrifuge. Decant through the same filter paper, and collect
& A5 g. {2 H7 j0 A# |1 _the washings in the volumetric flask containing the initial extract.: S- w" W M& b, n) O
Repeat the entire washing process two more times. Finally, wash the5 \& h; T/ g' \5 l4 o
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask7 ?8 S( K4 I% U1 g, k. h* e! C
to room temperature, dilute to volume with water, and mix.; H% ]* T8 p" ` m
Determine antimony, cadmium, and lead using an AAS/ICP-AES5 I* B2 U" o- N. c" E" S
technique appropriate to the specified level. Determine arsenic using the
* _- A) B5 {3 O o3 cICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
! ?: m8 ]* K6 K6 ?: |$ |& u& k4 vMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
: ?% t. K* N$ w/ N1 g. The selection of sample size and method of sample preparation
. g/ R2 B3 y$ w5 |; O- {4 `% J1 Emay be based on the principles of the methods described in Volume 4.
* D4 p" Q- i6 u) U% Y: |Aluminium oxide Reagents and sample solutions* ?7 E+ l/ f/ Q" e( |
0.01 N Zinc Sulfate
+ l2 ~. ~3 a( I! W) A: {- T9 kDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to* z& h6 p$ ?+ H) \; b+ ^! o
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg( ^+ T/ b0 u8 l7 w0 f0 u- r
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of7 x7 r" ]# @0 N6 [( z5 t* g
concentrated hydrochloric acid, heating gently to effect solution, then
* n5 J" P6 `3 L0 btransfer the solution into a 1000-ml volumetric flask, dilute to volume
1 `9 U7 e( ^7 n% zwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
3 H3 A/ i' _. yml Erlenmeyer flask containing 90 ml of water and 3 ml of
$ o8 ?- w1 j( zconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
% h ` a; i f. R8 G25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,. l6 Q+ a: t' S" u2 B- H7 k9 e; S
dropwise, ammonia solution (1 in 5) until the colour is just completely3 t3 D9 E/ w; P" P2 F, e. U' l
changed from red to orange-yellow. Then, add:" Y+ y5 x- ]9 z7 E- n
(a): 10 ml of ammonium acetate buffer solution (77 g of
* G9 J0 @4 Z* V/ uammonium acetate plus 10 ml of glacial acetic acid, dilute to/ \9 ~& Z8 H7 o& Y: S
1000 ml with water) and6 T" [* m4 Z! ?
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
- r m" K& V( z. k- qof diammonium hydrogen phosphate in 700 ml of water,
. P9 A. U# D. k7 O! H2 nadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,4 p) D+ {7 i2 ^7 R
then dilute to 1000 ml with water).
" V* P# ~ {8 i X- YBoil the solution for 5 min, cool it quickly to room temperature in a0 ?% b; }/ S! i3 E5 D% t# S; i
stream of running water, add 3 drops of xylenol orange TS, and mix.
- H* O6 `+ O* d cUsing the zinc sulfate solution as titrant, titrate the solution to the first
8 A( R" Z: K& }( U V+ x* Z4 dyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
; D4 D" v D j0 }) {/ Q* B, ^This titration should be performed quickly near the end-point by
/ N# T0 w, t2 e. D) nadding rapidly 0.2 ml increments of the titrant until the first colour2 v6 l5 [# _& l6 l1 r
change occurs; although the colour will fade in 5-10 sec, it is the true
- M4 e, d! Z" V+ Lend-point. Failure to observe the first colour change will result in an& ~- d6 U" M7 _) i
incorrect titration. The fading end-point does not occur at the second7 n7 u( ?0 _ h; O1 g- [ {- B2 A( M
end-point.)
% e( s# F/ A0 y% c% x/ [Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a ~+ | \9 n( H Q2 }
stream of running water. Titrate this solution, using the zinc sulfate
- e1 w6 F; Y0 z9 s9 L4 o$ t0 `0 i* n- xsolution as titrant, to the same fugitive yellow-brown or pink end-point
' a2 F9 j1 ?+ k# ]0 k) I# p% ias described above.
1 t) v3 P$ L6 ]Calculate the titre T of zinc sulfate solution by the formula:
, g3 M6 t- J* X% pT = 18.896 W / V
7 x: Z5 `+ q- F& J1 [( t% Iwhere3 I/ h, Y* {# H g" v8 w
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
2 ]/ n" T, c, d' R& H1 P# {W is the mass (g) of aluminium wire
- W+ ]0 d, J q1 D6 oV is the ml of the zinc sulfate solution consumed in the; F# G: u# t( n' q, e
second titration% w7 H! k0 }$ J* s: {5 p2 E7 L/ k: C
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and& {- H% B! F& a4 g( |6 ?* h2 w2 u
R is the ratio of the formula weight of aluminium oxide to
3 N' [- V; z2 h ~' `that of elemental aluminium.
/ o/ [: y+ U7 r$ }9 ^Sample Solution A
" a* ^0 o' p/ Q5 xAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
, c$ c$ m+ `. P5 Oglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
, ]) K" u) E. ^(Note: Do not use more sodium bisulfate than specified, as an excess
/ B* h D, w Rconcentration of salt will interfere with the EDTA titration later on in the! n, I: p r# I; W7 n8 {
procedure.) Begin heating the flask at low heat on a hot plate, and
5 }, \( A7 u6 i7 ?3 K$ Vthen gradually raise the temperature until full heat is reached./ E6 H2 ~! m) @, g" n
(Caution: perform this procedure in a well ventilated area. ) When
" P; |& a8 [, R$ |5 Rspattering has stopped and light fumes of SO3 appear, heat in the full, r9 @8 f7 F! g" [: j3 s4 N$ v
flame of a Meeker burner, with the flask tilted so that the fusion of the* }# Y/ N+ B8 W/ t
sample and sodium bisulfate is concentrated at one end of the flask.
. h5 u4 M `6 @9 m# \' aSwirl constantly until the melt is clear (except for silica content), but
0 f @8 }) r ?. S* E$ a% {guard against prolonged heating to avoid precipitation of titanium
' r( v e! d/ K+ ^6 a* Idioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
" o. A& K5 S" R* s) tthe mass has dissolved and a clear solution results. Cool, and dilute to
. p# |4 N- Y* q" |! f8 f! z120 ml with water. Introduce a magnetic stir bar into the flask." Z! M, @/ N0 ?
Sample Solution B
$ R4 E* ]: }& d- M+ WPrepare 200 ml of an approximately 6.25 M solution of sodium
# k% [! J& O4 [" g3 S3 Q# `hydroxide. Add 65 ml of this solution to Sample Solution A, while
+ O* y5 W% x; n1 _* bstirring with the magnetic stirrer; pour the remaining 135 ml of the0 s1 z+ V* W G/ A8 ], t! i
alkali solution into a 500-ml volumetric flask.
) p8 O( @ r: `" ]* ]6 uSlowly, with constant stirring, add the sample mixture to the alkali% }; J( M9 y2 J& S9 Z
solution in the 500-ml volumetric flask; dilute to volume with water,
1 k3 T5 _. y4 m3 Iand mix. (Note: If the procedure is delayed at this point for more than& l( Y4 b# _- b' n
2 hours, store the contents of the volumetric flask in a polyethylene
. A" u8 F& G% B8 n0 V/ Xbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
9 M2 a$ A. Y' @' Athen filter the supernatant liquid through a very fine filter paper. Label
3 O6 X7 j( I: a9 a! Sthe filtrate Sample Solution B." f3 F, \- o- ]0 B; u; ^$ ^1 ]+ j
Sample Solution C
; z# S- ^# ~. C' E, l: w6 kTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer5 p8 }$ h; x( S/ e
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid$ c' d3 N I# P
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
# Y! ^9 G) u K+ A& S# X) M0 V, h1 f) @+ NM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is0 u" J i3 N+ T9 H: Q2 t1 o5 F
known, calculate the optimum volume of EDTA solution to be added
1 L8 R7 i3 W( r* _: k/ ^1 jby the formula: (4 x % Al2O3) + 5.]
/ d! E- W, V3 q' tAdd, dropwise, ammonia solution (1 in 5) until the colour is just
8 {. }2 }* |3 }3 v& `, qcompletely changed from red to orange-yellow. Then add10 ml each z( `; \' _$ _$ p* D$ q3 W8 w6 T
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to" w9 Y6 m, `. G! z7 R$ F
room temperature in a stream of running water, add 3 drops of xylenol
5 @- @- _ c0 H# I5 Aorange TS, and mix. If the solution is purple, yellow-brown, or pink,
& W; U, v @/ b* v* Kbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
* e; ^" G( @9 y& ^" J) J3 S9 Y7 `pH, a pink colour indicates that not enough of the EDTA solution has
$ ]1 M+ V# L& u% E* ~; n5 kbeen added, in which case, discard the solution and repeat this
' T+ U6 x6 R, Y9 _procedure with another 100 ml of Sample Solution B, using 50 ml,
2 c* ^# B* ~ k* L% d+ o( nrather than 25 ml, of 0.02 M disodium EDTA.
2 F: l% j% ]" OProcedure
3 u( L7 l* W+ H8 AUsing the standardized zinc sulfate solution as titrant, titrate Sample
1 j8 }" `" S8 V7 o( }Solution C to the first yellow-brown or pink end-point that persists for
- k+ U a g, \5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first3 }& K o) Z, j4 B6 V$ ^) _
titration should require more than 8 ml of titrant, but for more accurate
6 W8 X6 V/ y- b; ^work a titration of 10-15 ml is desirable.
4 B* V C5 I7 yAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
, t) W+ _$ Y: A0 b& fmin, and cool in a stream of running water. Titrate this solution, using
t* O; _! G2 qthe standardized zinc sulfate solution as titrant, to the same fugitive
0 A6 Y% m. [5 i1 D/ B2 Jyellow-brown or pink end-point as described above.1 W2 O5 H) r8 j1 `
Calculation:
, c9 m+ D e) H+ e8 OCalculate the percentage of aluminium oxide (Al2O3) in the sample& w# j4 P# i9 Y7 ^* q, u" ~/ v
taken by the formula:
" H% x# Z! K# e+ g% Al2O3 = 100 × (0.005VT)/S
& N) X" P5 H8 I5 k. V" L W" ^where$ v9 x8 T- Q# {; w
V is the number of ml of 0.01 N zinc sulfate consumed in
+ ^( m7 @. c1 u% N& Sthe second titration,, T/ b+ ^( ~9 A- l# F
T is the titre of the zinc sulfate solution,
+ S( o2 J( h3 M/ v: lS is the mass (g) of the sample taken, and
$ H; l4 u! o2 p3 I9 G0.005 = 500 ml / (1000mg/g × 100 ml)., y( x2 r) W J8 q
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica( k s. f: g0 v# O6 o
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
) B& W4 q3 u, N& fHeat gently over a Meeker burner, while swirling the flask, until
9 ~2 ^6 z0 @6 m# ]* r6 Vdecomposition and fusion are complete and the melt is clear, except
# q4 {' m$ {9 S2 p* N9 M; lfor the silica content, and then cool. (Caution: Do not overheat the
! ]3 u8 Q# E4 W/ z; Ycontents of the flask at the beginning, and heat cautiously during
0 `0 U0 m$ ^1 o5 D5 q5 \fusion to avoid spattering.)! m' n7 O0 g$ D+ h4 ^! J
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat5 S% R( _! E# g
carefully and slowly until the melt is dissolved. Cool, and carefully add
% {( Z' }1 f6 _150 ml of water by pouring very small portions down the sides of the. w _( P: k. b- Z8 n' ~: c& G! x
flask, with frequent swirling to avoid over-heating and spattering. Allow
2 Y; U% B5 t5 b5 Wthe contents of the flask to cool, and filter through fine ashless filter( @8 ^. x/ ~$ @2 ]4 M" ~
paper, using a 60 degree gravity funnel. Rinse out all the silica from0 Q0 F* j+ p* q$ e& M
the flask onto the filter paper with sulfuric acid solution (1 in 10).
7 n- O0 L: J. ~0 i1 W$ X9 JTransfer the filter paper and its contents into a platinum crucible, dry in; N8 R. I1 H$ t* ]+ x
an oven at 1200, and heat the partly covered crucible over a Bunsen6 f" H6 Z7 _; D' J! k
burner. To prevent flaming of the filter paper, first heat the cover from
+ v% t: w4 O1 m1 f3 `above, and then the crucible from below.
1 u) P' H8 |2 P; xWhen the filter paper is consumed, transfer the crucible to a muffle2 w) Q. ` h7 [6 W, R( O+ Y
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and( p% b. d4 T# i# ]
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
" W, M9 n f" A- p( R7 ghydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
1 L4 \( A! m$ R& J: [. lon a low-heat hot plate (to remove the HF) and then over a Bunsen
% d* S! {' C( F* Fburner (to remove the H2SO4). Take precautions to avoid spattering,
8 g/ }$ H9 t4 R6 X1 Qespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a E o3 r& e0 t1 g7 c @
desiccator, and weigh again. Record the difference between the two
5 T( Z# L7 |6 ~ i# B' ~7 `) [+ Yweights as the content of SiO2 in the sample.) M6 i+ E; ]% Q% K9 j
METHOD OF ASSAY
6 ]; N! k _/ J2 y& H0 G" {Accurately weigh about 150 mg of the sample, previously dried at 105o
. J3 V: Y# @3 d/ h2 n! cfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
9 Z4 C4 |, \# l* z7 J+ Jand shake until a homogeneous, milky suspension is obtained. Add 30
. g4 o6 n, u7 y P3 Dml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
% y# l9 |. G0 H) }& {2 b zheat gently, then heat strongly until a clear solution is obtained. Cool,) a2 G# h2 e+ [& I! W5 E7 w& w* E
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
2 K- ~- P9 U- L- u8 Aacid, and stir. Add 3 g of aluminium metal, and immediately insert a2 ^- i3 Q# F V$ \6 ?7 X6 z5 ~7 o
rubber stopper fitted with a U-shaped glass tube while immersing the3 S# ~8 ?/ z& w( Z2 t
other end of the U-tube into a saturated solution of sodium# J! n9 u3 T+ Y, x# |5 z9 _
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
7 V7 v# N" v+ }5 whydrogen. Allow to stand for a few minutes after the aluminium metal7 z3 J, S j M9 ]1 H% m
has dissolved completely to produce a transparent purple solution.( u8 G; @* R1 X. S1 D! [$ l) z* S
Cool to below 50o in running water, and remove the rubber stopper7 Y# }/ m. r( w1 k8 U8 o
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate9 I" v+ b* X3 ]" l4 B, H% n* V
solution as an indicator, and immediately titrate with 0.2 N ferric
0 w$ q& \) o) p: s$ jammonium sulfate until a faint brown colour that persists for 302 j$ ^. [3 Q7 x3 }
seconds is obtained. Perform a blank determination and make any5 \' n' c4 ? {: }( h
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
5 _$ }5 B( U# ?( L5 S+ W7 c; Kequivalent to 7.990 mg of TiO2. q# b- ^7 W1 N; X6 Q4 o; r, {
|
|