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二氧化钛(钛白粉)
二氧化钛(钛白粉)
4 }8 P, _( Y/ K& I& W# ^ h
6 Q* V/ _/ B5 E5 {- ~8 ?' FJECFA关于二氧化钛(钛白粉)的结论! x" X- r N/ @+ O; S
; g4 U; g1 V2 \7 \+ }* q摘要: 2006年JECFA关于二氧化钛的结论" R) l2 }1 |" J: H
ADI值:不作限制。
+ @4 Z( c$ N" l" t& _0 Q: W# x功能:着色剂
' `# `" P2 N5 w1 w9 D
7 b8 E8 T5 r% \# z. H& FTITANIUM DIOXIDE2 Q3 P2 J0 g5 z1 Y# |* }
Prepared at the 67th JECFA (2006) and published in FAO JECFA! e0 x) l$ u' `; s$ ^
Monographs 3 (2006), superseding specifications prepared at the 63rd, t6 ^; S7 M3 q+ u( k9 T4 f( S
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the/ b4 V* `" `$ S0 {* J
Combined Compendium of Food Additive Specifications, FAO JECFA
( E( x2 M8 O- w9 n" ]" lMonographs 1 (2005). An ADI “not limited” was established at the 13th
r t0 Q* D* J$ o0 v) u. V) KJECFA (1969).
( |% e3 T& w9 {: ^9 E# R) T0 c( a! TSYNONYMS
9 j& S( y* w& t4 j( l* B9 aTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171& l- t" e+ y. d& D8 Y
DEFINITION
9 r& C. C3 B$ L6 vTitanium dioxide is produced by either the sulfate or the chloride @8 b8 F( S/ X) z1 R! o
process. Processing conditions determine the form (anatase or rutile
5 ^# Y/ g4 Z! O8 Lstructure) of the final product., t* d2 m1 a& ?, C e
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
6 O) X% s: a& U$ L# `* ior ilmenite and titanium slag. After a series of purification steps, the' p) ]* c1 S* Y8 X
isolated titanium dioxide is finally washed with water, calcined, and% c+ ~. i! u1 t) {3 R$ B2 h3 G- F
micronized.. i6 V6 K; v3 I" d9 T
In the chloride process, chlorine gas is reacted with a titaniumcontaining* [5 l, s+ o, C7 M9 l
mineral under reducing conditions to form anhydrous5 a+ l8 r# T1 j) A+ N: z& R5 a$ }1 i
titanium tetrachloride, which is subsequently purified and converted to
, Y* E, s! v9 R. M# Ytitanium dioxide either by direct thermal oxidation or by reaction with2 D1 U7 r2 s$ N |
steam in the vapour phase. Alternatively, concentrated hydrochloric
e6 E9 e* R$ ]! g+ d$ Q+ ~% ?- @, [acid can be reacted with the titanium-containing mineral to form a
* M% d) v; N* E. I3 X; F0 xsolution of titanium tetrachloride, which is then further purified and) E3 |2 D. B+ w n+ W
converted to titanium dioxide by hydrolysis. The titanium dioxide is
5 |& X7 l# b& n+ ]2 m) }7 V5 ifiltered, washed, and calcined." o1 u" i0 s6 X. Z0 p) d- b
Commercial titanium dioxide may be coated with small amounts of; G: N; t' v0 s4 r; l
alumina and/or silica to improve the technological properties of the
' s2 G- u4 n6 e* N) sproduct.# ~# R, x3 i! ?% b: j+ D3 ?; U
C.A.S. number 13463-67-7
* V9 h; x7 K, T* JChemical formula TiO2
; |) r2 T" c2 hFormula weight# l4 f5 h& l! K) Q6 C
79.884 ?! G2 P- m F- c
Assay8 H1 F3 K; x6 F& y: v2 U
Not less than 99.0% on the dried basis (on an aluminium oxide and2 ]3 B& I6 r: g0 C/ e( \0 r
silicon dioxide-free basis)
! j' G9 Q. x; h) \8 `DESCRIPTION
1 g! G4 w7 P' c6 n- l% l$ eWhite to slightly coloured powder1 p" v" W* r) `. F$ H" I2 u
FUNCTIONAL USES3 y2 R) R- e7 A* h4 @
Colour* E& `. Z M D
CHARACTERISTICS3 |! c/ }7 k8 W. O' r1 P) X/ c
IDENTIFICATION
' N5 @$ p% u% H+ DSolubility (Vol. 4)
- i0 h1 P9 `, s/ T) s6 S2 gInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
* d$ V9 V& i! @8 j0 l9 ]8 y$ Hsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
# Z% C U' z$ f% o7 k/ `sulfuric acid.
, ]* R6 I k- N) i2 j3 Y3 E4 VColour reaction
0 W4 k( D; s2 o! q r* i0 i: HAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
4 ~0 Y- D; B* w- [sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with, e) x/ b. c3 e$ X
water and filter. To 5 ml of this clear filtrate, add a few drops of3 D7 t" I/ m; a# q0 Y
hydrogen peroxide; an orange-red colour appears immediately.
+ n4 s# y. n% T+ ?( M& h; r3 nPURITY
" |4 J; u. k3 W5 q3 }Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h). r! }3 q/ i0 C3 e' \! Q/ v
Loss on ignition (Vol. 4)
2 ~0 J% S* d2 e6 w/ X. D1 aNot more than 1.0% (800o) on the dried basis) ?* t, |/ g9 L
Aluminium oxide and/or
0 X" |& h! h! w j# o$ p- a& }silicon dioxide5 M! U, i8 @& }) q3 y. j
Not more than 2%, either singly or combined
/ `. \* x4 A( t- ~; T( ISee descriptions under TESTS( z& _% r( A( y& z' ~& ~5 {
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
1 D# ^! L8 D5 M+ b$ Ralumina or silica.
/ h) K! v: F$ _& iSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
# F' X. ^% ~1 ^, Dplace on a steam bath for 30 min with occasional stirring. Filter
/ |* G+ ^7 U" Sthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
# d' y; d- G9 a) q1 G' Q9 l! |with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the) V5 B q# K- b3 d2 L/ O; H7 n
combined filtrate and washings to dryness, and ignite at a dull red# S0 v8 {6 i+ U8 Q- l* L
heat to constant weight.
9 X' u: b9 R# P2 |' ?" b# g [% [3 BWater-soluble matter
' J! e, N7 \) h# W" M0 w) @(Vol. 4)9 I8 R( Q! @3 l* Z; y" s. N4 J2 X
Not more than 0.5%/ k+ P0 a9 q, D A( F! d( h0 {& W
Proceed as directed under acid-soluble substances (above), using' c! l3 M8 ?2 c* e% O) _) Y
water in place of 0.5 N hydrochloric acid.0 B$ |# ~3 ^- n7 J
Impurities soluble in 0.5 N) F9 d9 ?8 u) L, l( @ `4 D& u
hydrochloric acid
. r) U: [1 v; I4 b/ ]Antimony Not more than 2 mg/kg1 T; S5 K5 N5 h$ ]% V# F
See description under TESTS# \# ]8 G' ^' X, v, L. _
Arsenic Not more than 1 mg/kg! @) L+ j; ^& h" s: c- O2 ?5 S- k
See description under TESTS
' }2 C. E6 [% X) Y/ sCadmium Not more than 1 mg/kg
- g) H# v6 P8 S( h8 aSee description under TESTS
; K# R& @. x2 v6 q* tLead/ W- q# i; L6 h% H9 u; D3 B8 W
Not more than 10 mg/kg
; v* K% R, J1 C# w" D) X8 ySee description under TESTS
* L, [1 `7 g1 y( f4 @, m' _5 `Mercury (Vol. 4) Not more than 1 mg/kg
z, l1 `4 E) M' l# r! `3 IDetermine using the cold vapour atomic absorption technique. Select a6 G" z7 a8 z1 {9 b. h9 R
sample size appropriate to the specified level
* C, k/ W3 ^: f4 k; e0 ^* PTESTS! [( w0 Z7 D b* f: f% K* b
PURITY TESTS5 }3 I: a; S& ]# D
Impurities soluble in 0.5 N: a) F9 \& m' ] V
hydrochloric acid
. p# S! G; I4 FAntimony, arsenic,/ q9 z6 e, P; X% s$ N; z$ `
cadmium and lead6 B' R# U& A* L
(Vol.4)% z% g4 m; v# e- ^
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N& I$ Z9 M7 n# E6 n9 J! ^
hydrochloric acid, cover with a watch glass, and heat to boiling on a+ \: r: P6 d9 l0 a( p4 A
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml( M; H: i( i* h; g& f5 M
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved: s \7 F; X! g0 m
material settles. Decant the supernatant extract through a Whatman
2 k$ S$ E$ ~9 V7 C+ QNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
4 v/ y! `5 H1 kvolumetric flask and retaining as much as possible of the undissolved
( e# A; v4 l' n( \: xmaterial in the centrifuge bottle. Add 10 ml of hot water to the original0 ]3 d- o$ w6 s! x u' L: ?7 z) n
beaker, washing off the watch glass with the water, and pour the1 T# r. D+ }' g7 k; L1 l% N7 A
contents into the centrifuge bottle. Form a slurry, using a glass stirring# }; r% ?: A9 b0 w8 G( l
rod, and centrifuge. Decant through the same filter paper, and collect
' J6 y+ }) X7 V/ \7 J( Q8 |8 ~8 _the washings in the volumetric flask containing the initial extract.
8 V! }2 Q; u0 v, CRepeat the entire washing process two more times. Finally, wash the
, l* i9 B/ X& P% F3 d+ Ufilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
# R( a p& b) g5 j# G7 Hto room temperature, dilute to volume with water, and mix.7 ?/ n% P7 {, \
Determine antimony, cadmium, and lead using an AAS/ICP-AES
7 a& G( K" @8 Xtechnique appropriate to the specified level. Determine arsenic using the
- I5 w: t' K& P2 Y8 y# w# AICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
x9 f- X2 D- v [( l. _Method II of the Arsenic Limit Test, taking 3 g of the sample rather than2 U4 _+ V/ N* [" y& d4 |% q; {4 ?
1 g. The selection of sample size and method of sample preparation
; [3 B6 H7 `5 Ymay be based on the principles of the methods described in Volume 4.
$ o- v2 v! H! t* e3 V: W+ A" RAluminium oxide Reagents and sample solutions
& o0 F' H# S/ x5 ~8 v% ^0.01 N Zinc Sulfate
: Y) b6 v2 Z/ K4 ]& aDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to; }- }7 f- m, V, h7 `* v
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg- h2 V9 w1 L2 v( W$ q1 W( |' i& |
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of. ]/ y. B" j# A: t4 x
concentrated hydrochloric acid, heating gently to effect solution, then$ y" C$ @* r; x4 |4 M) h- Z3 \ C; V
transfer the solution into a 1000-ml volumetric flask, dilute to volume7 S# h }# e7 K# y P
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
2 ?$ E, x e5 P. N+ `0 Eml Erlenmeyer flask containing 90 ml of water and 3 ml of
& L* Y7 S ~+ s' g; }concentrated hydrochloric acid, add 1 drop of methyl orange TS and; K: W( x" X s6 J3 M9 x9 r# X2 S) W; }
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
; l9 V: D" L0 ` b9 Hdropwise, ammonia solution (1 in 5) until the colour is just completely p" ?% M4 N( ^$ a8 H
changed from red to orange-yellow. Then, add:% U4 a, \' ]7 u) I' B) e2 p
(a): 10 ml of ammonium acetate buffer solution (77 g of1 Z- N* f; d8 o5 I
ammonium acetate plus 10 ml of glacial acetic acid, dilute to4 n( q: f+ _3 q/ A& Q8 e
1000 ml with water) and5 x/ q+ ]8 k. y% ]2 \2 E- n c) k
(b): 10 ml of diammonium hydrogen phosphate solution (150 g, ?. b3 c+ ]- K/ I5 i, S6 I0 P3 I
of diammonium hydrogen phosphate in 700 ml of water,# D8 ?0 L8 S& b
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
! m0 X& Z/ U' Z; Uthen dilute to 1000 ml with water).
5 @; ~+ ~, p. D, D/ x; N/ xBoil the solution for 5 min, cool it quickly to room temperature in a
8 k* W8 @; G" ^- x R+ \stream of running water, add 3 drops of xylenol orange TS, and mix.
5 S, U) |0 i, r& VUsing the zinc sulfate solution as titrant, titrate the solution to the first
& D5 I5 A4 f, w5 [" W# iyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:4 ]- T; S0 ]+ z: r( {
This titration should be performed quickly near the end-point by
! _8 {4 ~. C6 k" T) Q% D# D* Xadding rapidly 0.2 ml increments of the titrant until the first colour
0 g: H2 @5 s& T2 K# Y, s8 ?3 ochange occurs; although the colour will fade in 5-10 sec, it is the true: J) Z; }( o+ }/ _9 O7 B5 H4 A
end-point. Failure to observe the first colour change will result in an, c+ }" L/ v! ?- g% I7 Z% o5 b& B
incorrect titration. The fading end-point does not occur at the second
; b- [( A3 O) T6 e- _) d* Zend-point.)
' L) r- w, Z! |Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
4 V' z7 Z9 R) g2 W' M* O( zstream of running water. Titrate this solution, using the zinc sulfate
1 z$ w7 t2 X) b2 {8 hsolution as titrant, to the same fugitive yellow-brown or pink end-point- p1 C7 \& m# p/ C0 M, l
as described above.
& I5 r, F* V. G) z. rCalculate the titre T of zinc sulfate solution by the formula:
8 T, t( S8 k4 W/ G3 q1 x+ YT = 18.896 W / V' ?4 n& j9 P0 A' E5 q* ^8 c
where! S8 g" `+ W1 x
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution3 t1 `9 T9 M! E8 j7 Y
W is the mass (g) of aluminium wire& l/ @5 L3 t0 E& L
V is the ml of the zinc sulfate solution consumed in the
' O0 h- Y$ b8 ?4 V4 e: `' i: B Ksecond titration! N2 D5 F3 j( o; G+ u' ^
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
; `0 }0 L2 Y, L% G! p2 D: P2 h+ p1 lR is the ratio of the formula weight of aluminium oxide to( d; m: }( A/ u" Q$ o* W r
that of elemental aluminium. F0 R: f/ W; X
Sample Solution A8 U" e# A$ J1 p) P0 K) M4 D1 I4 j
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica, p7 \4 w! V+ Z$ {
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).. E# `# q" i, T
(Note: Do not use more sodium bisulfate than specified, as an excess
& j( E% O+ N' @. ]concentration of salt will interfere with the EDTA titration later on in the
! s) f" g1 `' eprocedure.) Begin heating the flask at low heat on a hot plate, and
# U7 i) j: v. V! t+ C& jthen gradually raise the temperature until full heat is reached./ Z8 N% z8 n4 F; H. T$ M7 b
(Caution: perform this procedure in a well ventilated area. ) When; h7 r1 V0 ]. a. B" }9 z
spattering has stopped and light fumes of SO3 appear, heat in the full' Z. P. R7 ~. a! h# J
flame of a Meeker burner, with the flask tilted so that the fusion of the
" v2 c. }1 Z& H7 p+ a! Dsample and sodium bisulfate is concentrated at one end of the flask.
4 U' `+ t4 W% OSwirl constantly until the melt is clear (except for silica content), but
) o! T0 D2 T- e' `. e# ~$ kguard against prolonged heating to avoid precipitation of titanium
7 d3 W$ d3 I2 {$ tdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until/ m. z8 r4 r( z4 a% i2 V
the mass has dissolved and a clear solution results. Cool, and dilute to# Z2 H6 P$ n1 O9 A/ W
120 ml with water. Introduce a magnetic stir bar into the flask.& j# U( R& f+ F$ S
Sample Solution B$ L g6 ~) T. C: }4 R6 s. \: j2 i
Prepare 200 ml of an approximately 6.25 M solution of sodium# I+ g U1 f3 c2 ?% x! P
hydroxide. Add 65 ml of this solution to Sample Solution A, while$ i9 V6 w& ~. [: x
stirring with the magnetic stirrer; pour the remaining 135 ml of the) e% W8 g& [# v8 m. Z; s
alkali solution into a 500-ml volumetric flask.. c( A2 O: ^' E
Slowly, with constant stirring, add the sample mixture to the alkali
3 u% @3 Z! c: H& P* ^' }solution in the 500-ml volumetric flask; dilute to volume with water,7 C8 a0 U9 g) [& r% O
and mix. (Note: If the procedure is delayed at this point for more than
0 A4 q$ W% y( Q% a2 hours, store the contents of the volumetric flask in a polyethylene
6 ~6 E. @2 s9 t. K& y, hbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),) U0 Z3 Q* ~3 m% B" p
then filter the supernatant liquid through a very fine filter paper. Label
* S" X" T B% o+ B, N6 i7 S1 ?the filtrate Sample Solution B.
6 f% r) G9 b PSample Solution C
9 G8 L' f1 ]' g. p4 V0 V: |Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer3 n Y+ J1 [. n9 [' ]+ z2 P
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid1 Q0 m7 J C( ?% k0 O9 V
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
. \- x$ i5 _( P: P% [: C4 rM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
{! g" K- l R% ~7 Pknown, calculate the optimum volume of EDTA solution to be added
: g4 S! I) S4 Nby the formula: (4 x % Al2O3) + 5.]% ]; M6 n3 F' b' A! d( P
Add, dropwise, ammonia solution (1 in 5) until the colour is just( o+ x( D' V R! |$ A- K
completely changed from red to orange-yellow. Then add10 ml each
6 q6 R' H% D) g( \& T; G+ E% pof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
4 _9 w; ]& e4 troom temperature in a stream of running water, add 3 drops of xylenol
. ]2 D6 ]/ |) s( b' rorange TS, and mix. If the solution is purple, yellow-brown, or pink,
7 o- c, B- I: x, | @- {bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
5 b! y: d, y; ^% q" npH, a pink colour indicates that not enough of the EDTA solution has
8 E$ z3 Z( r6 c9 @: c- [been added, in which case, discard the solution and repeat this
# h. A( L, ^) r' k- Kprocedure with another 100 ml of Sample Solution B, using 50 ml,
+ ?5 \$ D( }4 f7 b2 C( L% grather than 25 ml, of 0.02 M disodium EDTA.
6 K$ j5 V, ?9 j. A8 S. hProcedure/ u2 J1 n$ H1 F1 N7 j
Using the standardized zinc sulfate solution as titrant, titrate Sample
6 c: C' u7 Z! R% K" { Z- ]Solution C to the first yellow-brown or pink end-point that persists for) r- ?* d/ i7 j% x# U- S
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first7 Z4 o3 j) ~" [" V/ I4 w' f
titration should require more than 8 ml of titrant, but for more accurate% E2 \- F5 Z9 g9 \
work a titration of 10-15 ml is desirable.
4 l, R- `( V! `7 vAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
9 Q% I G8 j k5 k6 l. B) v Rmin, and cool in a stream of running water. Titrate this solution, using
% m' L' N4 ~' v1 _; V3 h; Lthe standardized zinc sulfate solution as titrant, to the same fugitive) R5 h3 c, E+ ?
yellow-brown or pink end-point as described above.
9 ^# f- m( Q" [Calculation:
n G/ B, N1 N# z8 s7 ]Calculate the percentage of aluminium oxide (Al2O3) in the sample; r' V, L$ ~& a* X; f0 T# f: C5 q' N
taken by the formula:
# U, p! @0 C2 v! f/ ~$ w: ]7 Z+ a% Al2O3 = 100 × (0.005VT)/S4 t3 ?) Q; y4 P, [5 I
where$ I; O2 B. V) F% [" Z
V is the number of ml of 0.01 N zinc sulfate consumed in+ T, s$ ^( L0 b& g2 J, J
the second titration,
8 Q' @ W* L5 R( D* k, b& dT is the titre of the zinc sulfate solution,& r! M7 f/ o$ ~% a: g! h
S is the mass (g) of the sample taken, and
5 d9 L4 U ]0 r7 R' M5 b0.005 = 500 ml / (1000mg/g × 100 ml).$ O0 \& L" `, H! ~
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica$ _+ O- K4 C3 h+ y5 u
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).% i& v+ I3 S2 Q; T- M
Heat gently over a Meeker burner, while swirling the flask, until
5 T- V) z; |4 G! b3 fdecomposition and fusion are complete and the melt is clear, except# G- u. t$ R1 p+ k8 L8 `% q
for the silica content, and then cool. (Caution: Do not overheat the
5 \! x9 B( i% d! Bcontents of the flask at the beginning, and heat cautiously during
- V4 U' q- L7 Bfusion to avoid spattering.)
% y/ C; j! Y0 c8 n' R: K- ?5 B+ CTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
" e0 U. E0 b- g: ]# F0 t& ~" V7 _carefully and slowly until the melt is dissolved. Cool, and carefully add
8 w/ H( D; H) @; b* B2 t1 K7 e, g150 ml of water by pouring very small portions down the sides of the* X7 b' p. b& F- T- P# H* l- t4 ?$ T
flask, with frequent swirling to avoid over-heating and spattering. Allow
1 m# b) Q3 P/ ~7 F8 [0 Wthe contents of the flask to cool, and filter through fine ashless filter0 E: ^4 D' r L
paper, using a 60 degree gravity funnel. Rinse out all the silica from
$ R4 C) S5 z4 l% |6 k! a, e6 q0 ]! Mthe flask onto the filter paper with sulfuric acid solution (1 in 10).6 O+ B: ?$ ]1 i, D' v. Y
Transfer the filter paper and its contents into a platinum crucible, dry in
+ C( c* b7 M! r$ G6 j$ y% F& a& Oan oven at 1200, and heat the partly covered crucible over a Bunsen8 h6 W/ d- Y2 d$ i, P! A
burner. To prevent flaming of the filter paper, first heat the cover from" G4 Q; g/ s u+ `5 u) K
above, and then the crucible from below.
! T+ x, z. q- q7 |6 f$ r/ VWhen the filter paper is consumed, transfer the crucible to a muffle0 K8 Y0 o" ]/ @$ j$ Q
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
; ^. T4 C' m b3 I" Z& rweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
k l8 t" B% w( ^7 ^3 Whydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
% Z o$ o1 n3 C! v2 A6 K, l. s3 son a low-heat hot plate (to remove the HF) and then over a Bunsen
0 P, r0 g5 R8 D# B0 J/ E, Rburner (to remove the H2SO4). Take precautions to avoid spattering,
8 k6 b0 T& m1 h, I4 m! w5 Vespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
" |0 B, ^; d# ndesiccator, and weigh again. Record the difference between the two. L% }4 l3 }" \" [$ _
weights as the content of SiO2 in the sample.
! {; {7 O: q; s3 aMETHOD OF ASSAY3 h5 m4 v4 C6 w) S! M/ F; d+ I2 m
Accurately weigh about 150 mg of the sample, previously dried at 105o/ Z7 X4 m- G0 P9 ]0 v& U* F
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
8 s5 V: b+ p/ `0 S# K7 \7 A$ rand shake until a homogeneous, milky suspension is obtained. Add 30 i; z5 v- Z, q c1 a% p
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially1 w7 o. E3 h/ ?% M; n* ]
heat gently, then heat strongly until a clear solution is obtained. Cool,& j }' W i) P, O) U( L# ~
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric& C0 D6 `+ B( C' l2 J3 w1 r# k1 H' M
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
) J) f7 C: U0 a( ^ @rubber stopper fitted with a U-shaped glass tube while immersing the1 O( U" e! I, t V+ w G# n
other end of the U-tube into a saturated solution of sodium
4 J8 m! P- m$ U) ]' }1 ]! ?bicarbonate contained in a 500-ml wide-mouth bottle, and generate$ y0 S. y5 x" Z2 |1 I
hydrogen. Allow to stand for a few minutes after the aluminium metal
* W: x4 N T. r0 O; xhas dissolved completely to produce a transparent purple solution.
: a# Y2 d0 l4 v& E2 H6 fCool to below 50o in running water, and remove the rubber stopper
0 Y- P6 B3 @5 Y: S6 y* R9 Dcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
. K% Y3 e9 ?6 \5 Asolution as an indicator, and immediately titrate with 0.2 N ferric
/ e+ h( N- i: a3 {7 S7 a" rammonium sulfate until a faint brown colour that persists for 30
1 h7 Y% h7 \8 q2 `seconds is obtained. Perform a blank determination and make any
$ [. x( F# l q2 z) Knecessary correction. Each ml of 0.2 N ferric ammonium sulfate is F) v! x3 l, q) X3 {) H* b8 J
equivalent to 7.990 mg of TiO2.+ d& B; `$ `2 O) I0 D
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