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二氧化钛(钛白粉)
二氧化钛(钛白粉)
# u; t2 }0 W& B6 g: ]9 A7 w! U- J6 c2 C3 ~: I# ]
JECFA关于二氧化钛(钛白粉)的结论7 G) P! _3 v6 M2 N
; F5 o: o' N) A摘要: 2006年JECFA关于二氧化钛的结论
7 B# U3 ~$ ~( D" a3 g' rADI值:不作限制。& U* R! c' p% b$ r) Q/ _- E
功能:着色剂: m. X% V5 o; d4 S3 `7 U2 w0 D
+ U7 B2 b/ v# Q8 y# @( ~3 v
TITANIUM DIOXIDE
# X( U+ F" i, @8 E$ ~" s- mPrepared at the 67th JECFA (2006) and published in FAO JECFA
* \7 G, m+ p0 ]* S5 v, O) bMonographs 3 (2006), superseding specifications prepared at the 63rd! f% h- D2 d9 [* ]3 ]
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
$ d6 z# b! `- a, [% k& HCombined Compendium of Food Additive Specifications, FAO JECFA
: x: o% @9 Q( f& W4 w& hMonographs 1 (2005). An ADI “not limited” was established at the 13th5 j9 w9 ^2 A( y* `4 c; o5 Z( S/ W
JECFA (1969).
( {3 t+ F3 K$ p4 X; }SYNONYMS; A5 c; `. ?) X+ Z
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171, D6 @1 w. S/ i( Y3 d) [
DEFINITION
6 R+ i9 \0 p" L: B4 W5 B" g) CTitanium dioxide is produced by either the sulfate or the chloride
6 j- F) d3 m* ?- Y' P# Uprocess. Processing conditions determine the form (anatase or rutile
% ~" b- A. d' w4 l6 {$ Pstructure) of the final product.
3 _( l/ z8 s1 kIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)% b+ v# x$ V3 n1 X
or ilmenite and titanium slag. After a series of purification steps, the
$ K9 m7 m2 c+ P: V4 uisolated titanium dioxide is finally washed with water, calcined, and3 a( a3 o9 B9 ?6 [+ {- |& i
micronized.- u" s ]% R6 a [. C7 u, D! J
In the chloride process, chlorine gas is reacted with a titaniumcontaining
. R4 x# f+ t8 P: Mmineral under reducing conditions to form anhydrous. I( o5 D" N7 W* [- B0 S) m* Q& x
titanium tetrachloride, which is subsequently purified and converted to) {6 J( u; f7 I2 L d; K
titanium dioxide either by direct thermal oxidation or by reaction with
- B( V. t1 [) i, ksteam in the vapour phase. Alternatively, concentrated hydrochloric
) J7 ~2 B9 V) C( |7 n# f+ Cacid can be reacted with the titanium-containing mineral to form a
- f- V; _7 r/ L4 j$ esolution of titanium tetrachloride, which is then further purified and
% u! q% e! [+ A3 d2 }! @& Zconverted to titanium dioxide by hydrolysis. The titanium dioxide is* r1 J' S9 I/ W4 {+ N
filtered, washed, and calcined.
* @* M2 e3 H5 X; G1 q: r; vCommercial titanium dioxide may be coated with small amounts of7 u+ }, m2 m7 @( @8 s
alumina and/or silica to improve the technological properties of the
0 y6 u3 m# l/ B- ?product.
8 x5 j* A! T2 l4 hC.A.S. number 13463-67-7' z- U. U& G0 V5 R% {% R' v8 y3 G
Chemical formula TiO2
, S2 o) i. I, H9 S5 c- uFormula weight
8 ^% _' ]5 B7 b8 Y79.88; z" A$ v' c% x4 M
Assay/ E; B$ H5 Z+ [% b$ L
Not less than 99.0% on the dried basis (on an aluminium oxide and
, N4 y+ @/ ~# C$ t! ]/ K. Rsilicon dioxide-free basis)
) `! P8 v& [6 `( _( F) UDESCRIPTION2 V2 h' Q0 ?' b1 P
White to slightly coloured powder
/ Y- m2 R* J3 |7 {, g7 SFUNCTIONAL USES3 _0 E. Q2 p% @2 K
Colour
/ c( o8 S% G! CCHARACTERISTICS
7 X1 G: h( B! n" d. {$ tIDENTIFICATION( u' p: Y" k& o* @
Solubility (Vol. 4)0 u0 }- x% V& q, Z: L6 z( d# S
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
! D; c& U" D7 E5 vsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated: _" M) b, W. ?+ V6 ~( Y, O- j4 P& _
sulfuric acid.
1 N+ _6 S0 i* c$ ?7 uColour reaction
2 Q8 ?: k# I7 r6 v( C& I! jAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
9 W! {% R9 `( I$ K( Q" Xsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
6 }- o. ] U: o4 u6 Wwater and filter. To 5 ml of this clear filtrate, add a few drops of
4 E& D8 C1 Y: O, ~9 R6 K+ }hydrogen peroxide; an orange-red colour appears immediately.
3 j; F4 _5 X) H6 C$ B0 ?/ ]PURITY. w m6 B5 Q1 G0 U+ Q/ G
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
0 r( p: g% E* l1 u$ wLoss on ignition (Vol. 4)
8 q3 A5 n# \4 n/ F! x& `" RNot more than 1.0% (800o) on the dried basis
' Q1 A3 s4 @1 V5 {8 M& ?Aluminium oxide and/or) ~8 ^. D' J' N
silicon dioxide
- o5 H5 |8 x- L9 SNot more than 2%, either singly or combined
/ C4 R. s3 w1 a# b1 [5 mSee descriptions under TESTS3 [1 K0 t. a: j1 }& U
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
- ^1 v d/ k" X7 jalumina or silica.
6 ~* {" j( U1 u# s; YSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and. T7 u, Q8 e! B, W0 F
place on a steam bath for 30 min with occasional stirring. Filter
1 \+ t" }5 b+ V0 l4 `1 D9 O4 Fthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
; T8 Y3 L( n5 N' g v* @with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
* k2 L+ n' n" A' u5 a& icombined filtrate and washings to dryness, and ignite at a dull red: w4 N8 S- C* f# Y; I! j* Q
heat to constant weight.' z2 F' R/ T& `, M* l/ X; Y/ e
Water-soluble matter$ A$ f: }4 e+ P, D
(Vol. 4)# p2 q" i7 O3 b! w
Not more than 0.5%: ?; k" V* b7 S
Proceed as directed under acid-soluble substances (above), using9 |& f. [6 n( h0 Y% |5 m" p
water in place of 0.5 N hydrochloric acid.
$ _/ J9 W6 I1 h8 K' aImpurities soluble in 0.5 N
' O" ^& d: B' z3 o% nhydrochloric acid* j9 D2 V% J5 p2 F& i1 C" u
Antimony Not more than 2 mg/kg6 N' h; v" `$ d1 S' o
See description under TESTS2 ] C5 w9 ~; t5 l y
Arsenic Not more than 1 mg/kg
& y, |% A+ O W4 q! N9 pSee description under TESTS
+ n ]3 X/ l( n5 xCadmium Not more than 1 mg/kg
. T+ L% a3 r& lSee description under TESTS
6 V0 b' z7 l* G; z- }Lead/ i0 m& q, \" N) u$ f7 K
Not more than 10 mg/kg
9 n- m- `5 r) U1 y9 Q0 [ R2 v: ~/ o( v* ^See description under TESTS
' s6 \9 W) t# ~% EMercury (Vol. 4) Not more than 1 mg/kg
& b4 E; Y( O3 d' }, uDetermine using the cold vapour atomic absorption technique. Select a
, O, S8 D0 y+ ^- C5 q( J$ Q& p& _, m6 m. Vsample size appropriate to the specified level( H+ ~0 j: H& J& Y1 w! J S/ G& ?% j
TESTS
# u1 h0 i& I0 m5 [ R2 O$ }% B4 d9 dPURITY TESTS+ O; |% T! n h+ i! g5 D" Z
Impurities soluble in 0.5 N
* x0 n5 H0 |- S6 ^' Bhydrochloric acid$ m' e- |$ A7 \4 ~/ K1 c2 @
Antimony, arsenic,1 d' m; [, [, I- t. u+ V
cadmium and lead
* b0 w3 C/ c! Q/ k(Vol.4) A' O! C2 t- n$ k; n
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
& M; o2 ]" O1 \9 S, s4 S+ \hydrochloric acid, cover with a watch glass, and heat to boiling on a- _/ M! j8 y z7 o" X5 a- Z
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml" q D7 a* x0 ]8 |9 P7 U& H1 {
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved8 [+ f6 n, m! h6 e: v1 Q
material settles. Decant the supernatant extract through a Whatman S- v# t' G$ J% m
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
, u, P/ U9 q0 mvolumetric flask and retaining as much as possible of the undissolved
" F5 P6 ~+ E, y" R/ Lmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
& C# k4 u1 C4 k' ~1 @1 {beaker, washing off the watch glass with the water, and pour the
1 }+ c& f/ e3 z W% rcontents into the centrifuge bottle. Form a slurry, using a glass stirring
7 T1 X3 u$ d" wrod, and centrifuge. Decant through the same filter paper, and collect
( z8 Y1 F, r7 N7 h, S$ x4 K) Vthe washings in the volumetric flask containing the initial extract.9 \; k7 z+ [$ Z( u. ` C' `
Repeat the entire washing process two more times. Finally, wash the$ f; V, o A2 j# D" [8 y. v3 z
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask% M! N% G% ]; O: D9 b0 l& P
to room temperature, dilute to volume with water, and mix.
% H5 s; m+ d. T6 I- G; D" [Determine antimony, cadmium, and lead using an AAS/ICP-AES9 I' T; t% h& ] H( }6 u1 [* H+ V" _# ^
technique appropriate to the specified level. Determine arsenic using the
' w1 d2 U/ [* w; [4 ^1 p' pICP-AES/AAS-hydride technique. Alternatively, determine arsenic using4 v( Q- T& ^2 _8 F+ `" ]
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than g$ v! ~' i$ {4 n
1 g. The selection of sample size and method of sample preparation
8 s" E' B" f' c, wmay be based on the principles of the methods described in Volume 4.0 [2 M! H) l1 o1 b0 X6 F
Aluminium oxide Reagents and sample solutions" Q7 F, C: M/ c
0.01 N Zinc Sulfate
5 i5 b+ T# d2 X8 A- v9 UDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
% l9 r+ v: e3 ]" ~; j6 pmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg B9 o8 i! z0 y+ G4 A1 `
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of N. Q' Q) b5 Q; e. q
concentrated hydrochloric acid, heating gently to effect solution, then
3 k1 b( ?8 u6 D0 Ntransfer the solution into a 1000-ml volumetric flask, dilute to volume
# c3 ^, d! t) |with water, and mix. Transfer a 10 ml aliquot of this solution into a 500( d' o. J" A4 v3 w. o
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
3 s" `! Q4 H/ o2 Q( \9 U$ D9 n3 yconcentrated hydrochloric acid, add 1 drop of methyl orange TS and0 f* z/ D( s2 d. U. y* a1 m4 M u
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
# l( q: M! o4 r M" jdropwise, ammonia solution (1 in 5) until the colour is just completely4 S+ ?$ E9 F/ q) r
changed from red to orange-yellow. Then, add:
( X4 X0 ~( R: h0 ?1 h& d4 Q, L) x1 u(a): 10 ml of ammonium acetate buffer solution (77 g of q4 T, F/ {# q3 v: B2 B
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
& |& A A; ^# [1000 ml with water) and
2 `$ P; }/ h& y9 |% E @- p/ P(b): 10 ml of diammonium hydrogen phosphate solution (150 g
- x, R7 m5 |% P# W: a) @: Q kof diammonium hydrogen phosphate in 700 ml of water,
; S3 M4 y3 z# v; Nadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,7 `! U' v7 T1 G
then dilute to 1000 ml with water).
# Y: U5 @9 E; o h. V$ k# BBoil the solution for 5 min, cool it quickly to room temperature in a
: r5 S' Q4 E5 u$ ~stream of running water, add 3 drops of xylenol orange TS, and mix.
/ U& f! C* c6 H5 hUsing the zinc sulfate solution as titrant, titrate the solution to the first7 H$ L8 {4 j2 ~! P$ d- S5 K
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:/ w2 P$ K# S ^* j/ ]; s& H
This titration should be performed quickly near the end-point by
! w$ q; |' n2 @/ padding rapidly 0.2 ml increments of the titrant until the first colour
& T1 { D+ h7 N$ A- b# ]# Schange occurs; although the colour will fade in 5-10 sec, it is the true3 N$ x P8 |5 B# m
end-point. Failure to observe the first colour change will result in an1 x E- D/ R* C
incorrect titration. The fading end-point does not occur at the second
7 j& o& x$ K1 Mend-point.)
) n: a" x/ K! s5 ^0 I8 hAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
' ~7 C- t, L) |# ^* F8 {- Ostream of running water. Titrate this solution, using the zinc sulfate
, n; z @# E3 y8 e4 j# l, }solution as titrant, to the same fugitive yellow-brown or pink end-point
, q' _# b* g5 Z5 pas described above.6 C. \' y5 `, C
Calculate the titre T of zinc sulfate solution by the formula:$ `# l S8 m2 n" Q( l- j
T = 18.896 W / V9 Q) ?, ]+ }( b# O' q5 o; n! s
where/ w7 R; M' u) b* B V7 G
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution5 I h+ ~) f/ g! w
W is the mass (g) of aluminium wire
: [1 f. k# _0 J" N( `8 `4 uV is the ml of the zinc sulfate solution consumed in the0 @7 P% k" K. U5 M% {, W3 C) W" x! u' G
second titration) T8 I- ?% U6 g, b+ G2 i( X) Z
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and5 ?: N6 t* `( S! {* n0 U( z
R is the ratio of the formula weight of aluminium oxide to! B: `/ ^' v# g. q) P4 h3 S3 N
that of elemental aluminium.
0 m; q6 g- w5 F p* HSample Solution A/ g$ F* `; C9 V) R; b2 n6 ]# [
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica5 m: y6 A7 J- j9 [/ m1 l- N
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).3 D" f. V+ [8 }; }% H( a- D8 g2 z
(Note: Do not use more sodium bisulfate than specified, as an excess) C, ]& `. x, V* Z# S% R& M
concentration of salt will interfere with the EDTA titration later on in the& ]' t' h2 s: }. i* A: e
procedure.) Begin heating the flask at low heat on a hot plate, and
6 L; b7 y' @2 G4 xthen gradually raise the temperature until full heat is reached.
$ Z0 k/ H( c- f7 S# ]) b' K/ x" r(Caution: perform this procedure in a well ventilated area. ) When
8 h& |! U) M: e S9 m% \( ^1 Cspattering has stopped and light fumes of SO3 appear, heat in the full
& s3 V, z' W4 A# cflame of a Meeker burner, with the flask tilted so that the fusion of the: M" ], m( B, T- Q
sample and sodium bisulfate is concentrated at one end of the flask.- q" F, f5 q8 Q3 f
Swirl constantly until the melt is clear (except for silica content), but
5 r( z; i8 h4 Rguard against prolonged heating to avoid precipitation of titanium
& p' K0 \% G: ]dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
6 z+ B( e& j3 p: s$ Ythe mass has dissolved and a clear solution results. Cool, and dilute to9 i2 _" g$ K' o4 a
120 ml with water. Introduce a magnetic stir bar into the flask.
. B6 h4 p3 s8 n( ^7 l# p3 vSample Solution B
9 @+ V: p! W+ h# o# u& S$ XPrepare 200 ml of an approximately 6.25 M solution of sodium
( ]( |8 {# \: W0 }/ k# W) a5 V! yhydroxide. Add 65 ml of this solution to Sample Solution A, while
4 O, F% o- q1 ]2 [; p$ u r3 hstirring with the magnetic stirrer; pour the remaining 135 ml of the
& `4 H8 C7 z) L3 h) I$ E2 Ialkali solution into a 500-ml volumetric flask.8 P7 r7 s. s( g H$ \
Slowly, with constant stirring, add the sample mixture to the alkali. \) C6 m4 z9 q" x
solution in the 500-ml volumetric flask; dilute to volume with water,
e& v8 F! B$ A- }: V4 ]and mix. (Note: If the procedure is delayed at this point for more than$ C$ J' O* V' }7 G
2 hours, store the contents of the volumetric flask in a polyethylene2 h: n& k2 @) c7 v$ p
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
/ S2 X! m- d( N& w# W6 Gthen filter the supernatant liquid through a very fine filter paper. Label& e, ~/ e" r0 V0 G5 U% U
the filtrate Sample Solution B.
8 ~3 K* b8 v) s! aSample Solution C
( d% r+ ^+ V3 W% UTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
+ J) o; S0 |, w9 d1 G8 m' Qflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid3 k# s9 R9 X7 j c
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
( Z7 q1 l/ Q v- F& E0 CM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is$ E; E% T7 m$ g) ^
known, calculate the optimum volume of EDTA solution to be added5 ]" d# a5 ?# g
by the formula: (4 x % Al2O3) + 5.]
+ Y J- d/ \' I" ?' F9 @Add, dropwise, ammonia solution (1 in 5) until the colour is just" y. v6 `: ?5 @* U5 Q
completely changed from red to orange-yellow. Then add10 ml each3 ~/ h& B8 R0 u/ h8 j
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to8 Y/ C, {! ] [
room temperature in a stream of running water, add 3 drops of xylenol1 q% S4 b+ v* ]+ ~/ d4 e
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
6 C9 Z6 _ Y& {' \' b# t; L3 Xbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
% x: C' I" x: H) P* p) Y, G6 }2 { lpH, a pink colour indicates that not enough of the EDTA solution has1 i$ m" D) e% C
been added, in which case, discard the solution and repeat this
, `" J. [4 _* p, Y+ `# \8 Uprocedure with another 100 ml of Sample Solution B, using 50 ml,1 B" y0 P2 A% b4 ]7 V! ]
rather than 25 ml, of 0.02 M disodium EDTA.
/ K) V* ?2 B) i; Z( v6 UProcedure% C! Z% ]( w: t v' Y/ |) q/ A9 ?
Using the standardized zinc sulfate solution as titrant, titrate Sample
9 h# |2 ^1 y) `" h% jSolution C to the first yellow-brown or pink end-point that persists for
- Y, U& w5 l0 D; N1 d1 x5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
) K8 Z5 n. y3 [) e9 xtitration should require more than 8 ml of titrant, but for more accurate- ~: A6 a" U6 E5 j: l/ E
work a titration of 10-15 ml is desirable.6 P5 D/ d8 s# |" B* M% b
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5/ X" I( \% W: C( ^* ]. h
min, and cool in a stream of running water. Titrate this solution, using/ W3 B- X3 k& s5 X
the standardized zinc sulfate solution as titrant, to the same fugitive
6 B: y6 {4 ?: O- r- i. E. Dyellow-brown or pink end-point as described above.
- ?: h) R8 B6 Q0 S5 T8 dCalculation:( A' R" R2 J8 P0 b" y3 E
Calculate the percentage of aluminium oxide (Al2O3) in the sample O3 D: N( @5 A8 x9 T# f0 g+ d& ?
taken by the formula:9 C2 ], r; Q& [( V
% Al2O3 = 100 × (0.005VT)/S
1 K2 O8 t' H5 q* ^! h3 p) xwhere
& M' f2 f: @9 j- ~+ P( l5 m% ]V is the number of ml of 0.01 N zinc sulfate consumed in5 R6 f. l2 J7 K) l, ^, g) M
the second titration,% ~2 }$ |3 O4 {) s: C1 e
T is the titre of the zinc sulfate solution,5 Y2 U4 E- [$ q+ E$ H
S is the mass (g) of the sample taken, and9 F/ d% d) B3 d/ o9 G
0.005 = 500 ml / (1000mg/g × 100 ml).; v+ _; x: s5 P% r) w9 v
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
: ]' D4 {0 ?" {# Q; tglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).! @4 L# q" f6 o# ?8 i5 y7 M
Heat gently over a Meeker burner, while swirling the flask, until
2 I& F8 {! e' g+ M$ y3 h, C0 Sdecomposition and fusion are complete and the melt is clear, except
2 j' P! Q4 f$ X5 z8 B; Bfor the silica content, and then cool. (Caution: Do not overheat the9 D3 A& Q. x5 G) h
contents of the flask at the beginning, and heat cautiously during
+ u+ b1 k, B8 v! v; k; U' hfusion to avoid spattering.)
) F0 H4 |& [+ S$ L0 QTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
|' D( v3 W: L* S, o- ncarefully and slowly until the melt is dissolved. Cool, and carefully add
- |- T4 ~* o# x$ f+ K1 I5 D150 ml of water by pouring very small portions down the sides of the0 c" R% O9 u6 E/ k) `
flask, with frequent swirling to avoid over-heating and spattering. Allow
3 u7 o$ @* }7 b( t0 e0 Zthe contents of the flask to cool, and filter through fine ashless filter
$ X& @0 K9 A* N! q( Z; n3 K4 Npaper, using a 60 degree gravity funnel. Rinse out all the silica from
7 V; ^' K0 D) M, }6 q6 othe flask onto the filter paper with sulfuric acid solution (1 in 10).
0 [3 P" M1 |) [& B1 _' W* pTransfer the filter paper and its contents into a platinum crucible, dry in3 U( f: m. C& ?. V* B
an oven at 1200, and heat the partly covered crucible over a Bunsen9 a& W- @# \; `. @3 G
burner. To prevent flaming of the filter paper, first heat the cover from! j( @, y% |* K' L% _/ k
above, and then the crucible from below. U5 e# [- O# ^5 X$ F
When the filter paper is consumed, transfer the crucible to a muffle
5 K0 |5 c. N7 ^6 }3 qfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and) F& `+ l' i$ E8 g; B
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
' i/ i" h! B5 I$ f; X7 m" X# Ohydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first; i7 G5 z4 \6 d/ q' l. r8 B
on a low-heat hot plate (to remove the HF) and then over a Bunsen
7 k1 h" p( M* S# U* Zburner (to remove the H2SO4). Take precautions to avoid spattering,
8 m7 z$ J( |$ f+ O, |especially after removal of the HF. Ignite at 1000o for 10 min, cool in a8 Z/ b& q! o R( [
desiccator, and weigh again. Record the difference between the two; k* L! N! u2 r$ Z8 }
weights as the content of SiO2 in the sample.
+ Q/ Y9 k A# ?METHOD OF ASSAY" n$ B- @2 j0 q
Accurately weigh about 150 mg of the sample, previously dried at 105o$ @: e% a8 v" l. _$ x/ V/ V
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
& [5 E3 X- ?- h) \1 B* k6 @and shake until a homogeneous, milky suspension is obtained. Add 30
- j/ Y1 ~) d4 e Q$ v2 Rml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially+ J9 G* h& a# a9 V5 v2 J" I
heat gently, then heat strongly until a clear solution is obtained. Cool,
# s) s3 z: F- a3 ?6 _then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
4 e5 s2 ]% n5 {$ \acid, and stir. Add 3 g of aluminium metal, and immediately insert a
" z3 C3 {5 f! urubber stopper fitted with a U-shaped glass tube while immersing the( l8 P. M% u/ n" H& V$ N7 x( _: S- H
other end of the U-tube into a saturated solution of sodium
9 L" u! N* a- n# L2 c6 jbicarbonate contained in a 500-ml wide-mouth bottle, and generate
. E0 G$ m, z, z, Bhydrogen. Allow to stand for a few minutes after the aluminium metal
4 t6 G$ j/ N1 U$ `has dissolved completely to produce a transparent purple solution.
8 t' [/ @( l8 S' p$ gCool to below 50o in running water, and remove the rubber stopper( ]9 E4 g" g4 q* _
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
& i G3 t% g# v; Y5 k. ssolution as an indicator, and immediately titrate with 0.2 N ferric# D' m2 `" X2 o' k
ammonium sulfate until a faint brown colour that persists for 30
% e$ L- S& m4 z N! zseconds is obtained. Perform a blank determination and make any ~0 p+ J& K5 n
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
; Q+ O F$ @2 uequivalent to 7.990 mg of TiO2.
6 K! c- i5 e" b |
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