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发表于 2008-5-23 12:10:00
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二氧化钛(钛白粉)
二氧化钛(钛白粉)
5 g; L0 ^9 e4 B% k! e& g+ a
4 i u! k: Y x( z2 [0 n8 B/ i5 iJECFA关于二氧化钛(钛白粉)的结论
+ V9 ~3 M' H' L0 I6 |# j9 }( [/ u5 U; E: h% V
摘要: 2006年JECFA关于二氧化钛的结论! V4 a! r0 C3 W P1 C) X: P0 v4 k
ADI值:不作限制。. D; `$ G, w0 Q) Z
功能:着色剂
' Q4 k! a- J/ D$ a* @! @1 F& G$ a$ v5 w
TITANIUM DIOXIDE) g0 |# T& u5 b' ?3 z4 M" a4 y5 G
Prepared at the 67th JECFA (2006) and published in FAO JECFA
, r+ j9 p( K1 W$ n; Q) JMonographs 3 (2006), superseding specifications prepared at the 63rd) F3 ?: G" m0 D* n
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the# L9 A" ?" M; u
Combined Compendium of Food Additive Specifications, FAO JECFA
. Q8 P& A) g# N3 l$ C+ }Monographs 1 (2005). An ADI “not limited” was established at the 13th
8 ^4 Y5 i i: N; @0 H: [2 ?0 u. K/ AJECFA (1969).. e* ~) j$ Z9 P" q
SYNONYMS. b! u& [: l" s* N8 w/ K
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171; }; A2 p, v- s1 s2 ^4 [: m+ A4 T1 I
DEFINITION& @' R. A( _5 Q, d0 A2 ^$ x
Titanium dioxide is produced by either the sulfate or the chloride4 G/ s9 ^! X5 ^ k& v$ c+ H1 P
process. Processing conditions determine the form (anatase or rutile
e3 b% U: }, O; W; |. s0 Dstructure) of the final product.* s, W* K+ I" _+ F2 S( n3 n' N
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
' y. m* x$ G. C; Lor ilmenite and titanium slag. After a series of purification steps, the
5 q E6 o" R; J$ }isolated titanium dioxide is finally washed with water, calcined, and
1 k6 h4 |7 c i, ^! }+ T2 `4 xmicronized.; }! ~/ I7 {9 h! d/ f# j
In the chloride process, chlorine gas is reacted with a titaniumcontaining) K6 \2 v) e$ \3 c z, k
mineral under reducing conditions to form anhydrous* O5 h1 i2 c1 }& i
titanium tetrachloride, which is subsequently purified and converted to3 d" I7 K. F# l6 w
titanium dioxide either by direct thermal oxidation or by reaction with% ? I7 k; J/ @6 D# I. ]
steam in the vapour phase. Alternatively, concentrated hydrochloric7 q5 V4 ^. n: S9 S, Z
acid can be reacted with the titanium-containing mineral to form a' M5 x# V2 o1 D
solution of titanium tetrachloride, which is then further purified and
& M3 N: w( W" iconverted to titanium dioxide by hydrolysis. The titanium dioxide is
2 f& F6 _2 S8 A, `- J/ P- zfiltered, washed, and calcined.
1 F# O; K$ I* c* \2 M4 C0 _1 U; s; ]Commercial titanium dioxide may be coated with small amounts of
- @) ~5 S; Q! f0 `alumina and/or silica to improve the technological properties of the& E+ U$ V0 s$ u5 e% }4 _6 E
product.+ _2 f# Y' y, I7 `1 k8 i0 e
C.A.S. number 13463-67-75 t- ]$ {" U* E8 P* q
Chemical formula TiO2; q! N3 I N" W5 m5 P0 N/ K
Formula weight! E, f# ^. d9 w5 j
79.88, c. g4 f, j& y0 t% S1 K0 t: Q
Assay- u% c% w, d. m+ U! k. F" s
Not less than 99.0% on the dried basis (on an aluminium oxide and7 T+ e. H6 F' F N' u8 Y6 m9 h
silicon dioxide-free basis)
1 w7 M' w# t9 _4 T1 ?& F8 u) w+ pDESCRIPTION# E: Y# a: q6 Z5 a: g
White to slightly coloured powder5 f9 I9 Z V* V4 Z
FUNCTIONAL USES5 \, o! o& U6 u. U5 e1 h: [
Colour
- ]4 v5 I" a* o: f7 b2 x/ {+ ECHARACTERISTICS
4 z1 @( n. |. |- p3 |& vIDENTIFICATION( ~/ \* D% r4 k8 k. {
Solubility (Vol. 4)& n2 g& j7 Q; d; {6 E* `
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
/ l+ e* i: H% g* j3 asolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
* [7 a( D, E8 w$ p% @' Usulfuric acid.
( \9 a3 |6 V" C! u5 x/ f x3 j$ qColour reaction V5 X; m, {* r- Q6 C7 J
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of+ G" ?6 d- S, G& f* t
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
( Q/ b7 Q+ h5 V" ]7 m! P6 H5 Rwater and filter. To 5 ml of this clear filtrate, add a few drops of4 Q! n% J/ X/ v, ^ V9 o' X
hydrogen peroxide; an orange-red colour appears immediately.% ]) n, {, d6 h G
PURITY
7 l/ _. X6 K v T @; t! r8 R! o! ELoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
3 C2 F. e/ W* x0 N+ d* w" FLoss on ignition (Vol. 4)
2 [& f- M& ^: ZNot more than 1.0% (800o) on the dried basis9 D0 ?1 w8 k; G( h, k' `# z( B
Aluminium oxide and/or y8 A& d( t* S
silicon dioxide# G$ A( y* E! W* x
Not more than 2%, either singly or combined
$ ?. T' C9 B0 c3 oSee descriptions under TESTS" d( I8 q& [$ K* a% d& r8 H
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing" I' }! d* J$ I; x
alumina or silica.
4 V7 @' r" M5 Z' V1 ]3 a: p YSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
' o) g: R# E @& ^: Z& yplace on a steam bath for 30 min with occasional stirring. Filter) _: B% Y8 ~8 `& |$ I8 b7 |
through a Gooch crucible fitted with a glass fibre filter paper. Wash b# \3 ~& |$ K: \
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
3 |3 u4 K/ C5 s9 [* _# m$ jcombined filtrate and washings to dryness, and ignite at a dull red
4 a; q$ E6 x7 lheat to constant weight.5 `, v9 ]1 C3 l+ T$ {/ L! ?
Water-soluble matter! z& d' O T0 g+ ]7 _1 U7 E
(Vol. 4)
$ a- z1 ^2 E# X( l" tNot more than 0.5%
9 O( T7 c# F4 |/ n4 v6 J. F& oProceed as directed under acid-soluble substances (above), using! |! Y A6 p. D% X* I
water in place of 0.5 N hydrochloric acid.
1 t6 _6 G. r/ T. MImpurities soluble in 0.5 N; R/ R( ~$ i' E& _/ H- o- O
hydrochloric acid
1 b0 V7 K' n1 _Antimony Not more than 2 mg/kg
3 M) G( M+ F# i. j7 i) z' a6 ~- q: eSee description under TESTS
3 V" o+ D; O' e3 V( C% LArsenic Not more than 1 mg/kg
1 C7 {. k: x3 A2 ^# ]See description under TESTS! k& a! |4 |; _: m ?+ p8 W
Cadmium Not more than 1 mg/kg1 _4 M6 f8 O$ N. q
See description under TESTS9 @9 h% B- e/ A; [2 {5 y9 X# c
Lead
1 O W! W; M* u/ n, o$ l: x: HNot more than 10 mg/kg: k9 [; D) j' T
See description under TESTS1 t0 A3 v7 ~& C3 A4 v) H, l
Mercury (Vol. 4) Not more than 1 mg/kg7 p/ }) i* b; F2 X. S3 P
Determine using the cold vapour atomic absorption technique. Select a% e# D& _! f& v3 D7 v2 ^( Z4 L* K
sample size appropriate to the specified level* S& {! U' t3 Y' N; n, V0 I
TESTS
/ c* ], e5 q. S- K, F1 J% gPURITY TESTS
0 v- E" K2 ~- p5 S' oImpurities soluble in 0.5 N8 r1 p; s' N9 b0 D5 _
hydrochloric acid: H; m8 M) S+ X/ y# h+ M
Antimony, arsenic,# {& b2 l; n) F- C. o H# \
cadmium and lead) A- p! T% ~: x; M4 a
(Vol.4)
( b+ N) Q! a4 f0 qTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
6 S7 K/ S+ ?/ q0 G8 }; whydrochloric acid, cover with a watch glass, and heat to boiling on a$ u+ o3 K6 ~% X( ^( Z1 o, y
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml! R; F( u: y# }5 w7 q5 u
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
8 |4 [' @! i! A2 y3 d" hmaterial settles. Decant the supernatant extract through a Whatman
* q" ~+ l$ O+ ~No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml, k2 R2 v9 F, m/ ?9 @ Z5 T+ b
volumetric flask and retaining as much as possible of the undissolved
, S+ l# X5 p+ O3 Q; Amaterial in the centrifuge bottle. Add 10 ml of hot water to the original
+ r$ v* r/ E s) z$ nbeaker, washing off the watch glass with the water, and pour the2 L+ E) I# A% v
contents into the centrifuge bottle. Form a slurry, using a glass stirring
0 r) \& f- T. H( G) J% Yrod, and centrifuge. Decant through the same filter paper, and collect$ } P1 L; x8 D9 l/ ]2 j
the washings in the volumetric flask containing the initial extract.8 L4 d4 D9 c6 z
Repeat the entire washing process two more times. Finally, wash the
8 ]$ z* z; [3 T+ R8 C0 C0 Cfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask5 q0 x8 R" B: Q! @# I
to room temperature, dilute to volume with water, and mix. X% ?, F% L( s
Determine antimony, cadmium, and lead using an AAS/ICP-AES
8 c/ H2 F# [ W% S1 c: ^, atechnique appropriate to the specified level. Determine arsenic using the, J7 ^+ Q; h6 x. a9 @" @6 d
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using: W& n* [3 s: O* H
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
4 E7 m: f7 [( w* I* L# Q( n- r1 g. The selection of sample size and method of sample preparation0 h0 b S8 P: n- |$ }( r0 F
may be based on the principles of the methods described in Volume 4.
( K+ I4 W) i5 T& cAluminium oxide Reagents and sample solutions
m5 D6 ]) F. G9 M: }+ @" q0.01 N Zinc Sulfate
/ v( \ i0 x/ |8 Y( O1 u6 |Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
4 ^. Z9 N2 @) K h# P& [' }, u0 @make 1000 ml. Standardize the solution as follows: Dissolve 500 mg1 F, r# Z W) ^. P
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of4 l! O. [- J! N/ X8 j" }8 l5 h7 J8 s
concentrated hydrochloric acid, heating gently to effect solution, then
7 v# H# V6 O1 \0 S4 ^* Ttransfer the solution into a 1000-ml volumetric flask, dilute to volume7 @2 [$ m% l! ^ J0 y5 W
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500* V7 a" M' x) u& j0 f; k) y
ml Erlenmeyer flask containing 90 ml of water and 3 ml of1 I& L5 `7 l/ `$ K6 ]
concentrated hydrochloric acid, add 1 drop of methyl orange TS and' b3 Y- M w5 }* k5 U& M8 d9 M
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
! v8 P( R$ @/ O' U3 g: d+ gdropwise, ammonia solution (1 in 5) until the colour is just completely/ c# s4 `# E' d+ l
changed from red to orange-yellow. Then, add:* N# {; m2 \- s4 M/ X' f5 M
(a): 10 ml of ammonium acetate buffer solution (77 g of
* Y2 G7 s5 M$ kammonium acetate plus 10 ml of glacial acetic acid, dilute to
/ u. A( v/ {. s$ o$ T1000 ml with water) and* E# d9 S+ T7 _
(b): 10 ml of diammonium hydrogen phosphate solution (150 g- B" Q$ z" B! s# G2 B5 i9 v
of diammonium hydrogen phosphate in 700 ml of water,& c4 U8 z T6 p3 @3 W9 N& }- a
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,& \+ O2 Y7 I3 [0 h
then dilute to 1000 ml with water).
* K0 ]- J2 P0 q9 H; z1 sBoil the solution for 5 min, cool it quickly to room temperature in a
) B9 |' p4 m! W# E2 o5 ~stream of running water, add 3 drops of xylenol orange TS, and mix.
! P6 s% s: i8 h. K% bUsing the zinc sulfate solution as titrant, titrate the solution to the first
8 a& o/ q e! a, O" V: w. ryellow-brown or pink end-point colour that persists for 5-10 sec. (Note:7 b$ M2 y# c# e% E
This titration should be performed quickly near the end-point by
1 |0 x( S/ g" U/ m3 yadding rapidly 0.2 ml increments of the titrant until the first colour
1 A7 p' H+ }! D N) Qchange occurs; although the colour will fade in 5-10 sec, it is the true) m/ F/ B4 j( o9 V( t( {* y
end-point. Failure to observe the first colour change will result in an5 b! \/ e2 U$ ]- b
incorrect titration. The fading end-point does not occur at the second4 P* @) A5 h( A* S5 W p2 b P
end-point.)4 @: h' l7 x/ u( z7 d
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
6 W5 d9 c0 J3 m) X# Q6 K+ d5 mstream of running water. Titrate this solution, using the zinc sulfate0 ]( }7 B4 c# M7 `/ x
solution as titrant, to the same fugitive yellow-brown or pink end-point
$ [# E6 Z5 P6 _as described above.
. |/ \1 Z, b' Z+ \. PCalculate the titre T of zinc sulfate solution by the formula:# }; _! p m r0 L2 V
T = 18.896 W / V
1 w7 A' J) f6 h7 Uwhere- r- l, l8 X2 W$ \8 j* d; S3 A
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
8 ]( N7 y4 c! f6 c& x6 PW is the mass (g) of aluminium wire
6 P0 u0 I. p2 e* x* a0 S- }/ c cV is the ml of the zinc sulfate solution consumed in the! R: M( J4 t" {6 l% ~
second titration
1 R+ h- `7 U: q0 G: p2 R9 y8 J18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
8 Z" ]6 T3 T% U4 i) G' C5 G8 {5 `/ xR is the ratio of the formula weight of aluminium oxide to
3 B5 F# @: b3 K1 W: s7 \) Sthat of elemental aluminium.* y# I4 \) M! X/ S3 Z2 d4 K) P
Sample Solution A
0 `! a9 q. e/ fAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica0 W4 r l/ s' Q/ }
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).; t- ?+ p$ ~% `9 M+ _- `& w/ K( f; T
(Note: Do not use more sodium bisulfate than specified, as an excess
T- ^# s. V* y! _' }9 Zconcentration of salt will interfere with the EDTA titration later on in the% F1 K5 W% B4 O2 O2 P
procedure.) Begin heating the flask at low heat on a hot plate, and4 r. i) ]4 L* w. e1 u
then gradually raise the temperature until full heat is reached.
$ Q$ E. A, q9 D5 F(Caution: perform this procedure in a well ventilated area. ) When$ Y& V- A" B6 Y: K$ C+ z
spattering has stopped and light fumes of SO3 appear, heat in the full" I; L+ `) Q* g- ~
flame of a Meeker burner, with the flask tilted so that the fusion of the1 _! N3 U9 g6 m. k5 v0 o7 |% J3 r
sample and sodium bisulfate is concentrated at one end of the flask.4 \, ]3 ?1 _6 T ~6 [
Swirl constantly until the melt is clear (except for silica content), but# f9 z( j0 x$ m' E
guard against prolonged heating to avoid precipitation of titanium: ?) ?+ y0 t8 b; J
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until' B6 [& J8 O# ^( g. v# ?( \8 g
the mass has dissolved and a clear solution results. Cool, and dilute to" q# c% |% G8 z
120 ml with water. Introduce a magnetic stir bar into the flask.
. d V. p% e8 F1 J& Q# u& PSample Solution B2 I. D5 t$ k+ H% P! G' i
Prepare 200 ml of an approximately 6.25 M solution of sodium1 [/ w3 f/ y* z& f) R
hydroxide. Add 65 ml of this solution to Sample Solution A, while1 U! \% Q3 D3 n7 _5 z
stirring with the magnetic stirrer; pour the remaining 135 ml of the& e7 o7 w4 [9 m( v! x7 N
alkali solution into a 500-ml volumetric flask.
0 g; s# M8 g; CSlowly, with constant stirring, add the sample mixture to the alkali7 n: s( y: X" s/ Y; ^, [" k
solution in the 500-ml volumetric flask; dilute to volume with water,
# d; r+ x- p6 Uand mix. (Note: If the procedure is delayed at this point for more than g+ ]& r# O9 X1 {3 K
2 hours, store the contents of the volumetric flask in a polyethylene1 b Z) ^' B. d& E' T& N7 O
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
! J4 |6 v1 ^3 I5 H/ F1 E+ M* f0 Tthen filter the supernatant liquid through a very fine filter paper. Label* R# @4 m, |' ]' Z( V
the filtrate Sample Solution B., ~ V6 n2 D% S! r/ M* `
Sample Solution C9 l: D0 ~ K! A8 h @ V8 Q, S
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer) q: R* y0 N" o! j9 H
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid; U0 j: b$ M' e& ~0 {$ \. V
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02* Z. s' s) T) _ |5 Z! t( n6 S( e
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is1 s6 ~4 V. c) R( ?* C% }# J7 @" N3 v" Y, Q
known, calculate the optimum volume of EDTA solution to be added- _' Q5 }! V$ T+ i% ~1 A' [
by the formula: (4 x % Al2O3) + 5.]
/ g8 s2 g$ X& y! ?5 qAdd, dropwise, ammonia solution (1 in 5) until the colour is just
8 D- x) W; L4 Bcompletely changed from red to orange-yellow. Then add10 ml each
2 i# o7 U* |5 L+ G; @2 Y) lof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to+ Y: ?! ^, t1 F+ ^0 |4 B( a! d
room temperature in a stream of running water, add 3 drops of xylenol+ V7 H) a! F, R
orange TS, and mix. If the solution is purple, yellow-brown, or pink,0 O4 @( ]0 |/ i7 A5 z
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired' V9 a4 u* X' e! W" O9 o4 h
pH, a pink colour indicates that not enough of the EDTA solution has
5 d8 Y7 V! d6 C$ Bbeen added, in which case, discard the solution and repeat this
' {9 R$ ~5 c1 r# Vprocedure with another 100 ml of Sample Solution B, using 50 ml,+ x$ _, H7 m3 e4 b1 b9 f
rather than 25 ml, of 0.02 M disodium EDTA.7 J" X$ ]. G7 _
Procedure
6 m2 ~6 V1 @1 fUsing the standardized zinc sulfate solution as titrant, titrate Sample* B& S E8 `* ]( K, k! q
Solution C to the first yellow-brown or pink end-point that persists for
6 q! w2 @, e" N5 D5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
7 B; ^% L. v% @/ Y7 y0 C. O# rtitration should require more than 8 ml of titrant, but for more accurate
. N7 A$ M w% G, N7 |0 Y8 Wwork a titration of 10-15 ml is desirable.
0 J( X' m" R2 p0 T* oAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
! E* c3 _# F) J' bmin, and cool in a stream of running water. Titrate this solution, using
3 I B a# a% v! G7 `the standardized zinc sulfate solution as titrant, to the same fugitive% I3 |# s1 Z0 c9 K
yellow-brown or pink end-point as described above.5 g* V+ O: W3 y( f" Z* u0 i" O
Calculation:2 P2 h/ K$ T$ Q1 f. y0 K$ R9 P% O! |
Calculate the percentage of aluminium oxide (Al2O3) in the sample
: n5 p! K2 a" ]1 _" N$ R/ w) Ptaken by the formula:) G4 R0 `) h1 b9 j
% Al2O3 = 100 × (0.005VT)/S
0 O5 |* d3 g# F, l6 Z, @+ gwhere' W# F9 G3 ~6 p- t% t$ C' r
V is the number of ml of 0.01 N zinc sulfate consumed in
( _# b0 U4 t( ^; d/ Zthe second titration,3 U! x+ N7 w7 C
T is the titre of the zinc sulfate solution,
6 }. g1 j$ u+ U: JS is the mass (g) of the sample taken, and" x& n U$ _% ^, z# q4 w
0.005 = 500 ml / (1000mg/g × 100 ml).
5 u; o$ a2 C0 `Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica) R1 d) b( I6 z0 _# u4 H
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).$ @% x, P9 J# Q% l9 J7 @' x
Heat gently over a Meeker burner, while swirling the flask, until) e/ M/ d+ a' K, u% \/ w6 j) M
decomposition and fusion are complete and the melt is clear, except
# z+ H7 J) h2 B5 d$ ~( l5 hfor the silica content, and then cool. (Caution: Do not overheat the
" A- b! N }/ ?- }) econtents of the flask at the beginning, and heat cautiously during) ^& k0 ^" W5 r
fusion to avoid spattering.)
7 t! t- Q4 C& ?) s5 YTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat5 o6 W/ G9 Z! Y) x: l' A0 l
carefully and slowly until the melt is dissolved. Cool, and carefully add) Y+ o4 f; T: W& y k9 O
150 ml of water by pouring very small portions down the sides of the( W2 Q8 @4 b* ]7 M! b
flask, with frequent swirling to avoid over-heating and spattering. Allow
9 V# y1 ^* T. E$ Y0 Fthe contents of the flask to cool, and filter through fine ashless filter2 }3 ^' y1 c, z
paper, using a 60 degree gravity funnel. Rinse out all the silica from
# b; L' b v3 ~9 W3 vthe flask onto the filter paper with sulfuric acid solution (1 in 10).( z0 O+ W" H7 a8 {8 W1 R+ P. W
Transfer the filter paper and its contents into a platinum crucible, dry in
0 Z3 R, U6 a7 o8 C% d+ zan oven at 1200, and heat the partly covered crucible over a Bunsen. O O) G1 P+ I2 G3 m
burner. To prevent flaming of the filter paper, first heat the cover from
: |' {) S' }; p- ~, e) w# n0 Uabove, and then the crucible from below.3 z* l- r8 p ]0 k
When the filter paper is consumed, transfer the crucible to a muffle
& p! A8 V# |; R9 R5 |# `furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
% G8 p$ _; l7 o3 N2 C6 Vweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated5 Z! Y" N* \5 e/ Z" u& d: l
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first9 s. o, q7 S& t
on a low-heat hot plate (to remove the HF) and then over a Bunsen4 v6 C4 F9 b$ {# T' a3 ]* E
burner (to remove the H2SO4). Take precautions to avoid spattering,1 \: Q. ^$ K5 v. a$ O
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a% d% ~6 \' b% [ }( v+ V0 k
desiccator, and weigh again. Record the difference between the two3 r$ j _7 J' r: S
weights as the content of SiO2 in the sample.
0 n+ h, U; q6 Q$ D0 \& E' JMETHOD OF ASSAY
+ B( z/ I" q9 L: `/ l" mAccurately weigh about 150 mg of the sample, previously dried at 105o
2 g# e1 T/ |9 J" Ifor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water! j! d0 x5 A D0 X
and shake until a homogeneous, milky suspension is obtained. Add 30; ?( n5 y5 Y M: e. a) g
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially! x+ H. M1 Y) Y9 m! |. n
heat gently, then heat strongly until a clear solution is obtained. Cool,- R \- m+ g- q' W0 \; p, e: n
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
; ~6 E6 [' k& W' j: f! a1 C6 macid, and stir. Add 3 g of aluminium metal, and immediately insert a2 C3 z2 n, {# U
rubber stopper fitted with a U-shaped glass tube while immersing the5 d( ^: \( E: o) P( ?8 x
other end of the U-tube into a saturated solution of sodium! @5 d' ~ q! N. b! V9 }" F& o- X
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
& A, g) m4 ?$ Q( N, n& s& r& Q# p Whydrogen. Allow to stand for a few minutes after the aluminium metal
& f* S! ?9 B3 x5 bhas dissolved completely to produce a transparent purple solution.1 E. q/ w7 ^+ S" [
Cool to below 50o in running water, and remove the rubber stopper
: Y5 a1 a0 l6 K4 M( u* c: Lcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate0 U6 I9 P' O: {; T
solution as an indicator, and immediately titrate with 0.2 N ferric& ]2 G: a [4 {# e; |; R
ammonium sulfate until a faint brown colour that persists for 30
6 o# ^0 Z4 y0 x4 F. O3 b2 tseconds is obtained. Perform a blank determination and make any
' n! A. p. q& l; ?( K8 g; lnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
5 M6 e; ?1 ^) g8 x# \; fequivalent to 7.990 mg of TiO2.
5 ?: x0 y; ^+ a) F2 M |
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