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二氧化钛(钛白粉)
二氧化钛(钛白粉)
" ]- K7 x% E- @6 _& V
8 z3 }& D0 M: ^( I# x8 v9 ?+ iJECFA关于二氧化钛(钛白粉)的结论& z5 F! t( u0 S. o; z. X
0 a; P# M( X. K7 y
摘要: 2006年JECFA关于二氧化钛的结论
, ~% s8 G* s/ M) r0 eADI值:不作限制。
# k2 T7 v# s. C _8 r功能:着色剂
$ W( u# F$ z* e; m7 Y# u, T
/ f3 J! e% r7 L+ V7 }TITANIUM DIOXIDE7 ^6 M- ]/ z- U7 r3 g
Prepared at the 67th JECFA (2006) and published in FAO JECFA
G1 X& G' o. M3 XMonographs 3 (2006), superseding specifications prepared at the 63rd r; k( o" T) Y$ G) G; M
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the+ G0 m- {) x- k& Q9 B. N3 ` r
Combined Compendium of Food Additive Specifications, FAO JECFA
* c9 R. s: [! u$ ^! LMonographs 1 (2005). An ADI “not limited” was established at the 13th
: C- N; f; M" c. p- VJECFA (1969).
2 Y' b2 G, [9 l$ u: }( G0 _+ VSYNONYMS( V4 w# N7 ~3 h% ^) i, C
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
. H7 l7 E5 B" @9 P0 X& iDEFINITION$ q: p0 n* D8 e
Titanium dioxide is produced by either the sulfate or the chloride4 z( m V0 | B; I/ K
process. Processing conditions determine the form (anatase or rutile
( c, Y4 r( x2 G$ [structure) of the final product.
- s+ D K$ k. f( j/ c9 C5 FIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
9 Y- R- w2 o. ^% M; Lor ilmenite and titanium slag. After a series of purification steps, the
, m! I- G0 \' d& b- w) Gisolated titanium dioxide is finally washed with water, calcined, and
5 K9 m# F0 _% a# L1 I1 Tmicronized.8 ^, }+ ~ A8 p M. Q
In the chloride process, chlorine gas is reacted with a titaniumcontaining8 t& D6 J0 G ]
mineral under reducing conditions to form anhydrous
p3 Q2 @: E4 q2 h& |- K5 {! Ftitanium tetrachloride, which is subsequently purified and converted to
m8 z- V9 l- \, z, Z9 b) M3 ?# k' htitanium dioxide either by direct thermal oxidation or by reaction with6 V3 H- L9 s' a B7 s9 `( Z9 V
steam in the vapour phase. Alternatively, concentrated hydrochloric, L- }% a- q& `! x% v
acid can be reacted with the titanium-containing mineral to form a
8 R" S6 [) H2 _7 T( Psolution of titanium tetrachloride, which is then further purified and
: D& a- M+ d) j' y# v8 }. jconverted to titanium dioxide by hydrolysis. The titanium dioxide is
6 V8 `1 a( k8 y# Ofiltered, washed, and calcined.. C z/ X8 r/ B' j
Commercial titanium dioxide may be coated with small amounts of
1 g( O3 R7 d. J) f& Balumina and/or silica to improve the technological properties of the* t( C2 r7 S) N" u
product.
7 e! ]8 |, C2 m1 ?C.A.S. number 13463-67-7# x' E$ j+ f: N$ d
Chemical formula TiO21 O# p& s, }6 h' y; d, F# ]& l- k
Formula weight
3 s+ }" I$ w* A, c' m, H& ~ h79.88
" D- K6 R0 S* B. _Assay/ f$ N, Q" J1 ~5 }: ~3 J
Not less than 99.0% on the dried basis (on an aluminium oxide and2 e$ B9 ~1 P6 j" E$ f
silicon dioxide-free basis)# E$ \& Z9 W7 e! h; M
DESCRIPTION
$ @1 L- H4 I0 m/ E$ z+ g; [/ nWhite to slightly coloured powder0 A; e8 }! a% y% x- `
FUNCTIONAL USES- ?/ P# ~4 h; h3 h. O6 W8 o
Colour
# B5 V+ E) t$ o" ]' DCHARACTERISTICS7 S) |# y# M( o. |
IDENTIFICATION E0 i5 x, ]2 N! e/ x# y \5 D
Solubility (Vol. 4)
- v3 V$ k* }" aInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic6 W2 B" p/ C; H( |( h
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated0 \( b9 t/ J+ b2 ]+ H- K# n
sulfuric acid.
/ E f! M: p1 }Colour reaction
6 \% ^; v' t1 n5 iAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
' w; j% e E2 Ysulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
1 b& I6 K+ ^ _/ \8 v$ \, i7 nwater and filter. To 5 ml of this clear filtrate, add a few drops of& m3 g) i: Y) l8 y+ M& f
hydrogen peroxide; an orange-red colour appears immediately.9 u" h e/ C- d& c) u, j1 [/ t
PURITY* R+ O$ k( [: X
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)$ f7 F h9 ]* }. Q
Loss on ignition (Vol. 4)# f M3 x) n4 Q$ |% S$ z, K+ C
Not more than 1.0% (800o) on the dried basis5 V) ] \/ M( a9 {8 [
Aluminium oxide and/or" v4 M9 d/ m" Z: ^& u
silicon dioxide
9 [8 t1 a) G; m4 N. ?- wNot more than 2%, either singly or combined8 V; @9 R# S7 b! O$ x
See descriptions under TESTS- E- w8 p% \7 b; e4 O
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
: |: q3 D& Y9 u' ~9 n" f! y, Ralumina or silica.: [) i: \) K ?) V: F4 [
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and9 U) F6 q- ?* D. M: L
place on a steam bath for 30 min with occasional stirring. Filter/ E7 D0 |- W+ z- B/ f& ^, p) x
through a Gooch crucible fitted with a glass fibre filter paper. Wash
: `& V8 y6 T( wwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
7 ^ C5 m" C- c1 X. h Dcombined filtrate and washings to dryness, and ignite at a dull red! y/ @: Y5 B- ?5 X/ v2 J( U
heat to constant weight.
4 r% _4 V7 N6 v; {Water-soluble matter7 O4 y3 H/ \' d& Q3 C2 F2 W. u
(Vol. 4)
1 [9 A# ~$ C/ b3 Z+ g9 [% q! TNot more than 0.5%4 D2 Y/ T4 e4 h7 o
Proceed as directed under acid-soluble substances (above), using
. f: ]+ a: C+ u9 B6 mwater in place of 0.5 N hydrochloric acid.
% V" S, x- {2 z3 J% ^) X. ]Impurities soluble in 0.5 N
/ {2 F4 T6 o: O8 p5 |4 W" ehydrochloric acid
/ f+ }( Y i! k/ n& y+ V4 [8 rAntimony Not more than 2 mg/kg( m. t+ | y! d* R9 e( q
See description under TESTS
1 W/ K* Y( \& Z, O2 v5 [+ E1 wArsenic Not more than 1 mg/kg
& H0 y" K3 k2 A8 h% {See description under TESTS
- ~9 B4 w4 k5 J9 \8 bCadmium Not more than 1 mg/kg' A) k) V+ ^3 }* v7 e
See description under TESTS* \0 |1 i( j* B" k& b; Q/ i
Lead2 z0 m" E! ]2 K% i/ k& q
Not more than 10 mg/kg
& m% b$ q9 I* ~) ~0 C XSee description under TESTS
0 r! ~( b6 \9 y/ v3 \Mercury (Vol. 4) Not more than 1 mg/kg
2 N' I8 a5 a/ e* c5 b2 EDetermine using the cold vapour atomic absorption technique. Select a
& [7 ]5 _# H1 S( H) d5 lsample size appropriate to the specified level3 b5 a& P) d3 W
TESTS
2 _+ k6 O, d8 r! }PURITY TESTS2 }: d8 N: g0 g; ?4 Y( P! Q4 R
Impurities soluble in 0.5 N3 ^/ z( U6 t' G0 h
hydrochloric acid4 }9 i+ ?3 y$ p+ {
Antimony, arsenic,9 k0 p1 [1 w8 M) I5 [/ {- t
cadmium and lead
, T8 ~% q1 Q8 J) v* a# t(Vol.4)
# a: X7 |/ H T9 z$ q1 K* V- RTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
. k' O! w N' Y, yhydrochloric acid, cover with a watch glass, and heat to boiling on a, ~. a# A# e" U; b
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
+ R8 q3 `# R4 S( xcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
( |+ F0 W+ @6 i( ^material settles. Decant the supernatant extract through a Whatman
) C" e! T* v6 K* ~! b& l( fNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml2 g! u' E/ e: I" _( `
volumetric flask and retaining as much as possible of the undissolved: d& p! s$ Q5 r1 R9 [+ }
material in the centrifuge bottle. Add 10 ml of hot water to the original' f# a3 M9 L, X* l
beaker, washing off the watch glass with the water, and pour the
, }, S# s7 j/ R8 {! f8 i9 xcontents into the centrifuge bottle. Form a slurry, using a glass stirring
4 B# P0 m) ?9 D! W# W/ d( `3 d3 Zrod, and centrifuge. Decant through the same filter paper, and collect
$ z) c+ b2 l! m9 i) P! Ithe washings in the volumetric flask containing the initial extract.
& |+ a4 l$ ?9 s1 W G3 B5 L+ v3 s6 vRepeat the entire washing process two more times. Finally, wash the
g H" c/ m7 c5 x4 D. x+ |filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
! h* H% s! M" g; Z7 nto room temperature, dilute to volume with water, and mix.
6 p4 X/ Z; m# A- XDetermine antimony, cadmium, and lead using an AAS/ICP-AES; N0 y0 Q/ G i. {7 {' U$ q
technique appropriate to the specified level. Determine arsenic using the
9 z5 c4 \: \7 TICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
* I$ \$ l* m3 q2 U' h9 IMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than& H8 H! X# G: f- o! e* @3 W
1 g. The selection of sample size and method of sample preparation
: k" z S) G, ^6 A# S. imay be based on the principles of the methods described in Volume 4.2 w2 J# m; p- O* t4 w7 t
Aluminium oxide Reagents and sample solutions
1 U9 Z, [( c0 _3 i+ I' G0.01 N Zinc Sulfate
1 ~* a" ?, Y1 `' s- PDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to, f5 X+ i* y2 @; O, G( A! X
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg) m# }0 K1 S* C: \
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of- C1 z$ O! O1 u. s
concentrated hydrochloric acid, heating gently to effect solution, then
4 U& ^; X2 E, C" S+ Vtransfer the solution into a 1000-ml volumetric flask, dilute to volume; V+ R) w2 B. i4 B) X$ c" T; b- A+ v! M
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
, _5 B+ P0 i( G- p9 v) qml Erlenmeyer flask containing 90 ml of water and 3 ml of5 j8 C, B- B' j- `
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
" Z( ?/ x0 C+ F q% R25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
v# N& }. L: h4 s/ v" hdropwise, ammonia solution (1 in 5) until the colour is just completely* I+ B5 M6 j, q/ n7 E" R x
changed from red to orange-yellow. Then, add:& _1 Y' ~' Q! o: b6 \
(a): 10 ml of ammonium acetate buffer solution (77 g of
7 F1 E8 b( ~/ L; ?4 N' W; Y+ \ammonium acetate plus 10 ml of glacial acetic acid, dilute to
6 i8 i1 i/ H0 e# T- j" p1000 ml with water) and
- h$ r+ L) h2 m& L(b): 10 ml of diammonium hydrogen phosphate solution (150 g
/ E$ ~) L9 e1 B& N; R& O' pof diammonium hydrogen phosphate in 700 ml of water,' d2 x* g! i2 T" [% c
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,7 s. s) S- { ]7 x- ~' O o4 @
then dilute to 1000 ml with water).8 u" t4 N/ _: l' b7 ^& d
Boil the solution for 5 min, cool it quickly to room temperature in a
' e; P& m: ]; {9 g3 xstream of running water, add 3 drops of xylenol orange TS, and mix.
+ D( Z1 N. l% d$ d; U' \: ?5 ?Using the zinc sulfate solution as titrant, titrate the solution to the first' t& F& ^( d4 S' {: O: N5 p
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:8 U$ B7 t( \1 u
This titration should be performed quickly near the end-point by; D; O1 G5 Y; n; f3 j
adding rapidly 0.2 ml increments of the titrant until the first colour9 o- [ R {% F% G) \7 p( H
change occurs; although the colour will fade in 5-10 sec, it is the true3 [7 M8 ?+ g# t
end-point. Failure to observe the first colour change will result in an* ^0 r# a+ n+ W# l, Y3 p
incorrect titration. The fading end-point does not occur at the second& W% B+ X1 G2 l
end-point.)
4 R7 d: r. ] E+ y* }/ i0 w, m, cAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
1 D/ B2 q0 ?/ `8 Cstream of running water. Titrate this solution, using the zinc sulfate9 p8 q X8 m* I, q# A2 `$ E
solution as titrant, to the same fugitive yellow-brown or pink end-point# o* v9 C' ]! q! A! f3 X
as described above.9 \; x! g' Z6 a/ s
Calculate the titre T of zinc sulfate solution by the formula:9 q5 {4 H& ` D- g! h" C
T = 18.896 W / V( D) @& J M$ K& W
where
: v0 w1 Y5 T7 l- f: Z& m# iT is the mass (mg) of Al2O3 per ml of zinc sulfate solution" M0 W! `% h# Q5 m/ P! ?
W is the mass (g) of aluminium wire
) H7 {; u, V2 \/ z6 T. M/ RV is the ml of the zinc sulfate solution consumed in the
g8 |2 L3 |. _. P0 Tsecond titration8 `+ T& U" q4 _) n
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and( |- k! n% P/ f/ X( Y' S; n
R is the ratio of the formula weight of aluminium oxide to
6 ?8 B$ L! M$ W: o0 Mthat of elemental aluminium.% Q- E# G0 \7 ^# Q4 F6 H
Sample Solution A
1 I% M3 ~6 O9 o- ]0 f- VAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica% X( h' v* e% C8 x$ M9 j, ?3 [4 _6 v
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).9 K' ^) _; A8 `! T, s$ z' H
(Note: Do not use more sodium bisulfate than specified, as an excess
- S# c1 [) R' _, L3 w$ @6 U' Vconcentration of salt will interfere with the EDTA titration later on in the
* B- p2 S9 J( c; ^$ X, @+ \9 eprocedure.) Begin heating the flask at low heat on a hot plate, and7 s" \* U+ s+ o, @5 O
then gradually raise the temperature until full heat is reached.3 d8 `, S4 U, W3 M2 T: q" B
(Caution: perform this procedure in a well ventilated area. ) When! c X) u1 O0 n& V; [
spattering has stopped and light fumes of SO3 appear, heat in the full! J; B* k/ D+ X% o* G" p
flame of a Meeker burner, with the flask tilted so that the fusion of the
! V6 J1 ]5 H5 _. m; |' z) Dsample and sodium bisulfate is concentrated at one end of the flask.$ `# G8 y* U. |) E% B
Swirl constantly until the melt is clear (except for silica content), but
5 K l" d, s: iguard against prolonged heating to avoid precipitation of titanium
8 T$ e9 t C' ~! \5 E, Kdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
! C* D2 \3 D @+ e) Y$ n' g% ?& Vthe mass has dissolved and a clear solution results. Cool, and dilute to
% Q1 N" `0 Z+ s3 f; \8 ^4 O6 h6 m120 ml with water. Introduce a magnetic stir bar into the flask.8 y5 r# i8 {9 K7 `* ~1 p
Sample Solution B' R6 A7 y7 r9 d& W% H' V
Prepare 200 ml of an approximately 6.25 M solution of sodium1 u, q% W+ R( V- x
hydroxide. Add 65 ml of this solution to Sample Solution A, while9 A; a2 p, ~2 h
stirring with the magnetic stirrer; pour the remaining 135 ml of the; c& S$ _# b4 {$ `" x& O* F# t: T4 c
alkali solution into a 500-ml volumetric flask.! N9 I* @( a6 H4 M# Z& Y
Slowly, with constant stirring, add the sample mixture to the alkali
/ g ]5 `+ y9 \6 M# {: xsolution in the 500-ml volumetric flask; dilute to volume with water,
, f6 m7 `$ X. K8 r: tand mix. (Note: If the procedure is delayed at this point for more than
, d% P4 X( ~, _3 z0 B2 hours, store the contents of the volumetric flask in a polyethylene
9 H2 V; p' b+ A. \, B0 h& s- T% {bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
n1 E6 N' k3 Q- ~. _% ^, `& @/ c9 fthen filter the supernatant liquid through a very fine filter paper. Label$ E. T8 c0 h }3 X
the filtrate Sample Solution B.
3 w5 M( c" Q" c% K1 P& kSample Solution C
3 c9 R8 C- Z7 f0 Q2 G+ D9 {Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer! w$ a# p$ j% @0 q) F! u
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid# g! ~3 k1 ?6 n1 _$ l' a
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02$ L; l: x3 w: [' i4 e
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is( L! n) \0 ? r v8 v f$ v
known, calculate the optimum volume of EDTA solution to be added
3 v7 u$ T: \. [9 a; jby the formula: (4 x % Al2O3) + 5.]* w4 q6 |1 C5 t( o3 Q- J
Add, dropwise, ammonia solution (1 in 5) until the colour is just
2 C2 X. p% q) D6 X5 vcompletely changed from red to orange-yellow. Then add10 ml each
" t1 |) o) [- n. ?5 X8 C. V+ C- \of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to$ g- K: k# S: \2 j
room temperature in a stream of running water, add 3 drops of xylenol
# T: \/ R* N9 _! qorange TS, and mix. If the solution is purple, yellow-brown, or pink,0 v; Y1 p I" G3 [" i* @
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired* T2 s+ Z- J5 y/ _; m3 `; Q; S8 a
pH, a pink colour indicates that not enough of the EDTA solution has
, [5 _% f6 M% Q' S* {" Bbeen added, in which case, discard the solution and repeat this3 J: S1 |& I) I8 ^0 A; w- m( @- J
procedure with another 100 ml of Sample Solution B, using 50 ml,
7 O- Z7 Y" a' U9 \% V5 d- @, }- x& Grather than 25 ml, of 0.02 M disodium EDTA.2 Z1 ^6 e9 d5 [ I* Z# x
Procedure, O: E9 J9 Q2 a8 j
Using the standardized zinc sulfate solution as titrant, titrate Sample$ c7 o H& @/ O- P [' f" e
Solution C to the first yellow-brown or pink end-point that persists for
( n- p \7 \0 s7 L/ E% |, l: l5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
6 j( ^- ^+ {! ]+ }1 g5 k; atitration should require more than 8 ml of titrant, but for more accurate: Y/ E5 [' D! H: R; N B2 h
work a titration of 10-15 ml is desirable., D2 @$ h3 h( `
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-59 L+ [- V7 D2 T3 g
min, and cool in a stream of running water. Titrate this solution, using4 F, J6 E0 N( M" \
the standardized zinc sulfate solution as titrant, to the same fugitive
$ u2 z0 S% {5 Hyellow-brown or pink end-point as described above.
# z! q M6 u& z {6 @Calculation:. c+ _1 \+ x, S# k1 x+ x. Z
Calculate the percentage of aluminium oxide (Al2O3) in the sample
$ T2 s7 ?# ?2 h0 F- _* S8 ~9 Ztaken by the formula:
8 D& E3 l4 K5 g1 d1 f% Al2O3 = 100 × (0.005VT)/S
/ A, q; |+ w. Ewhere; W% k! ?+ d9 C1 w' @
V is the number of ml of 0.01 N zinc sulfate consumed in; t/ Q3 c( U& s+ @2 A8 r% N, R
the second titration,
3 S' |. b7 C7 ET is the titre of the zinc sulfate solution,
* B) H# e# `. n: {& |0 l$ o! aS is the mass (g) of the sample taken, and
' A5 F5 O/ E+ [' J' |0.005 = 500 ml / (1000mg/g × 100 ml).8 K# c2 F/ X* M; R; h
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica* R* Y! n+ h8 G V1 K- f! S6 F
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
: {4 N4 L. [% t* RHeat gently over a Meeker burner, while swirling the flask, until
2 w$ e+ n! z; u+ q4 _: u& c1 u$ Mdecomposition and fusion are complete and the melt is clear, except
" b+ @. x4 ?5 c# E+ A; K: I7 ufor the silica content, and then cool. (Caution: Do not overheat the
0 Y$ X3 }$ b2 Y% b7 U. econtents of the flask at the beginning, and heat cautiously during1 b$ b" ^( R& l8 \- u
fusion to avoid spattering.)
! e% j: \2 ?6 XTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
9 l8 B( R+ q$ W% ^( B. ycarefully and slowly until the melt is dissolved. Cool, and carefully add
' P# u( R+ G+ j# y' Z- b150 ml of water by pouring very small portions down the sides of the
* Q1 d% o+ w |+ S* aflask, with frequent swirling to avoid over-heating and spattering. Allow2 }3 W- s4 q4 Y0 ~4 x
the contents of the flask to cool, and filter through fine ashless filter5 M% L/ |5 R# x! v# n0 `2 ]
paper, using a 60 degree gravity funnel. Rinse out all the silica from3 s: N: r$ M& U" ?/ {
the flask onto the filter paper with sulfuric acid solution (1 in 10).
& l$ j4 w4 K5 X8 f3 {; L0 C, aTransfer the filter paper and its contents into a platinum crucible, dry in; N3 F2 G% `3 m G4 P! t
an oven at 1200, and heat the partly covered crucible over a Bunsen/ z. B. i- L4 i& `' b& k
burner. To prevent flaming of the filter paper, first heat the cover from
2 z9 R" C. j/ F3 J- _6 wabove, and then the crucible from below.: u- n$ ]; f N. J: B$ m
When the filter paper is consumed, transfer the crucible to a muffle& j1 A; e6 p) x% A1 _9 J% p- n8 [
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and. T3 T) {% @8 G( C6 N. a/ q- I
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
# D1 t6 c7 B0 I6 Yhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
( J$ z. F- y/ yon a low-heat hot plate (to remove the HF) and then over a Bunsen
: Y0 A' E8 ~) J5 kburner (to remove the H2SO4). Take precautions to avoid spattering,+ i9 ?) A) [$ b( d8 z
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
5 G5 r8 a* p4 C* H) R* R; m P/ `desiccator, and weigh again. Record the difference between the two% X9 v" s" B4 U- k9 A
weights as the content of SiO2 in the sample.
& Y6 [( e( B- S# z' CMETHOD OF ASSAY
. W6 R; C2 ^; p' Z, D2 f" PAccurately weigh about 150 mg of the sample, previously dried at 105o
2 C7 G/ u; x2 a. K& hfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water) R ^2 m7 f1 q, ^
and shake until a homogeneous, milky suspension is obtained. Add 30% H$ _; E; f9 Z4 a3 K+ b# r
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially* `- _8 Q5 t+ t: q/ p, X% p; r2 a7 G: d
heat gently, then heat strongly until a clear solution is obtained. Cool,, l7 T) `! Q# x: Z; x
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric' O# n' B |2 u8 u
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
+ b! M2 Q9 K) N- qrubber stopper fitted with a U-shaped glass tube while immersing the
$ ?- |7 D; @( ^, |$ B* H' x. kother end of the U-tube into a saturated solution of sodium% A# I! ]) y9 t2 V1 w
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
9 S" n& R6 ]0 h. M& ]* y* jhydrogen. Allow to stand for a few minutes after the aluminium metal
" t1 L3 ^4 i: [has dissolved completely to produce a transparent purple solution.
, K) D1 _4 z% n( S0 H4 J4 B) HCool to below 50o in running water, and remove the rubber stopper
9 n* {7 E* x+ bcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate! U- s, |$ j# X Z
solution as an indicator, and immediately titrate with 0.2 N ferric
. d% g9 I9 K9 I% n4 ?' H) N. Yammonium sulfate until a faint brown colour that persists for 30$ }) z5 q" l L( T T4 ?4 s: V, K
seconds is obtained. Perform a blank determination and make any/ y5 b9 l- K8 |$ A
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is/ w% N8 t C8 N$ B2 p6 f) T* J. Z
equivalent to 7.990 mg of TiO2.5 r$ u5 @1 X' x( Z# K; G& s
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