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二氧化钛(钛白粉)
二氧化钛(钛白粉)
: C- }* I6 R) a& y8 l/ ]& d: G$ W# x P4 ~8 Z7 }: ^
JECFA关于二氧化钛(钛白粉)的结论
. H( j: T! u% Y1 h0 B5 c* q. G. ~ `6 x5 [
摘要: 2006年JECFA关于二氧化钛的结论
, c" r4 E" R% ~6 u8 fADI值:不作限制。# @2 S% Q6 n* i
功能:着色剂
2 d5 T: Y" c( a8 j4 x. K4 _' @" Y8 A% b/ k9 V
TITANIUM DIOXIDE+ D. _( |' r; F! v2 ~2 X+ `
Prepared at the 67th JECFA (2006) and published in FAO JECFA
( T$ x0 \) Q4 iMonographs 3 (2006), superseding specifications prepared at the 63rd8 \: \; r- y0 B2 m* Y5 J" ]
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
& }1 l' M Y( C9 hCombined Compendium of Food Additive Specifications, FAO JECFA+ N' h. Y5 Y+ {& l8 z J; R( z
Monographs 1 (2005). An ADI “not limited” was established at the 13th5 J" `% o; T: j# i6 x8 P
JECFA (1969).- S3 s1 ^/ g5 _" |# F* e
SYNONYMS6 g. E& r4 E( O3 P9 c: R
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
# S" I. g$ {0 t( Q6 o! H; eDEFINITION7 \) F5 r3 s8 `- h/ s+ J. }
Titanium dioxide is produced by either the sulfate or the chloride
9 Y& T+ T$ }& Z" ^( z! b1 ]# Jprocess. Processing conditions determine the form (anatase or rutile( J' \0 C# z: A
structure) of the final product.3 }3 W9 @0 F( b, [5 K, K
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
* N a# }- B* a) Y% T$ oor ilmenite and titanium slag. After a series of purification steps, the' N; [% t `0 `0 l2 Y/ @! g) R
isolated titanium dioxide is finally washed with water, calcined, and
/ n' q' `% D; }9 O! ?1 B) B1 A' Smicronized.
4 W; q( T% v# e! M) I$ U f/ ~, AIn the chloride process, chlorine gas is reacted with a titaniumcontaining. z7 I: J1 ^$ i" v2 i9 V
mineral under reducing conditions to form anhydrous: j# t/ T0 m7 E2 j6 p
titanium tetrachloride, which is subsequently purified and converted to
% p- w$ y0 i" m& p, ctitanium dioxide either by direct thermal oxidation or by reaction with) U7 U1 \6 I( g& b
steam in the vapour phase. Alternatively, concentrated hydrochloric
. j0 G4 @4 O) a; I! x) y8 g) u( Hacid can be reacted with the titanium-containing mineral to form a
: K a# R1 r/ n. t; V: hsolution of titanium tetrachloride, which is then further purified and
& s0 l( E n- s) ]converted to titanium dioxide by hydrolysis. The titanium dioxide is
- }9 U' Q6 a% X# ]6 ?5 dfiltered, washed, and calcined.- ]0 d* u) V6 [8 r- |- h
Commercial titanium dioxide may be coated with small amounts of
( z* k5 Y+ r9 `: V5 Balumina and/or silica to improve the technological properties of the
* R4 q8 J; M7 ^" ]* Pproduct.
9 d1 V7 Y5 s2 K j/ x/ m3 vC.A.S. number 13463-67-71 a3 h& M0 l2 \) j( l* B
Chemical formula TiO2
5 _; n8 c+ J$ {- T8 q& I7 w$ SFormula weight
/ N+ \# H% n% I79.88
6 h* o: J2 B8 M% }+ y* x2 xAssay, K( [% T n3 y% a! H
Not less than 99.0% on the dried basis (on an aluminium oxide and
- F+ m, B3 X1 m2 ysilicon dioxide-free basis), y4 K0 P) ]% j4 O* X
DESCRIPTION
* t9 ~ [. j# x0 j; P# _- F' {White to slightly coloured powder
7 ^" F& Y- f" L4 @FUNCTIONAL USES' M' R( M0 R; |! j
Colour% c% T u& p7 E! I
CHARACTERISTICS
3 |9 Y" u0 j5 r$ N# |1 V0 W9 MIDENTIFICATION* v- A0 |! y' m* H+ ]5 s3 A
Solubility (Vol. 4)2 z% ]4 {" |/ D+ Q6 w! \9 R
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic, a" L( S' q- \8 g! u% N" u' k- U
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated- H9 `% y, ~1 x! T8 U" J
sulfuric acid.
5 L5 s8 p: {8 A, U8 u$ h4 ?Colour reaction
2 t B' v& t8 Y8 o HAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of! ~' R" H [: W
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
: Y( m0 d0 y. z) {6 v: e ywater and filter. To 5 ml of this clear filtrate, add a few drops of/ w- E' ^- }' r6 }( Z" U c; `9 K4 X
hydrogen peroxide; an orange-red colour appears immediately.
- e+ R6 J0 S5 m h# bPURITY' T. o7 a) I2 `% A! ?
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)! f* L- u/ h" J7 h5 w8 Y8 Z# O% [& Y
Loss on ignition (Vol. 4)
* I) L! C: A/ I l8 M' @1 X- ?Not more than 1.0% (800o) on the dried basis. D4 B0 f& ^) ^, Q
Aluminium oxide and/or
9 _3 W. @: h- D- m9 y3 h9 Q. l. jsilicon dioxide
3 w# D* h, h8 k6 A& L. [Not more than 2%, either singly or combined2 `& o/ l$ g/ K
See descriptions under TESTS
1 j( ~. q8 T7 u" l* B2 G. K5 pAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
7 V X% K: B# E) Q/ l% G( k2 B- aalumina or silica.( N/ h* v1 e* H# H1 f
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and3 C# }- j2 S6 m A' G
place on a steam bath for 30 min with occasional stirring. Filter
: S0 a% |. M9 U" B* o' Dthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
: M8 m$ K6 |0 x: R4 Q$ o$ T! Iwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the1 | D- H3 d5 ?6 ~3 d
combined filtrate and washings to dryness, and ignite at a dull red
2 d4 } f+ |& L7 X f, @heat to constant weight.+ V* c1 F1 X2 @8 N. {* D
Water-soluble matter6 T* |4 T3 F* b+ U
(Vol. 4)
! m s( |+ C2 j Z: d0 Y2 u0 [Not more than 0.5% r1 _( d. r/ C4 l
Proceed as directed under acid-soluble substances (above), using
, `, R4 }) F) x, ywater in place of 0.5 N hydrochloric acid.
8 Q2 K: T0 y) Z& B2 N: W' ~Impurities soluble in 0.5 N
+ X5 c/ i! P+ Y# A$ }hydrochloric acid. A/ S! B7 }. u j
Antimony Not more than 2 mg/kg
, D1 @" P; u1 o- Z9 `See description under TESTS
. Z0 d; z" g7 a7 JArsenic Not more than 1 mg/kg9 E+ l7 C+ Y1 B
See description under TESTS) A. I, h* h* K/ n7 O& X- ?( A; r
Cadmium Not more than 1 mg/kg
' |7 H& K9 D4 Q: j; d- G, B$ HSee description under TESTS
* @+ Z- }' s) WLead0 R* R$ g; B+ u# n; K; D5 V
Not more than 10 mg/kg$ ]2 k9 D8 U( n
See description under TESTS
2 a( f+ |2 |2 m4 x3 J7 XMercury (Vol. 4) Not more than 1 mg/kg6 i$ y# C. d& ]2 \7 q
Determine using the cold vapour atomic absorption technique. Select a
) R- s q5 O. ]& isample size appropriate to the specified level
! q, j* \. _$ G6 fTESTS
6 {) h3 h$ o, {) T. _PURITY TESTS6 \, F9 p! V" y% e
Impurities soluble in 0.5 N
: C/ ~. C" K; o, B! ~hydrochloric acid
& |, M, T4 ^" d7 I! G" h' AAntimony, arsenic,6 A& m+ p6 k3 `3 s7 m" P) }
cadmium and lead9 g; ?9 L. w+ V: u9 c: h
(Vol.4)
3 a+ Y. K% x/ ~0 s0 ?. T5 aTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N ~. }( Q; j+ J5 J# M7 o
hydrochloric acid, cover with a watch glass, and heat to boiling on a3 B j( @% k" F/ W+ `
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml! c3 [% A8 g/ \# ], q
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved8 R" K1 k2 p" S; `
material settles. Decant the supernatant extract through a Whatman" ]" K& Z' f# d$ d$ d0 W2 }
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml I, L+ @% K$ l1 |. _( J0 L
volumetric flask and retaining as much as possible of the undissolved
2 ?5 _9 f( m5 N \ a: gmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
* B$ ?- D* T7 {& a$ }$ C; k5 Cbeaker, washing off the watch glass with the water, and pour the* ~8 q3 ]/ u' ], R
contents into the centrifuge bottle. Form a slurry, using a glass stirring4 O1 w8 M( z. o
rod, and centrifuge. Decant through the same filter paper, and collect
) S; F0 A Y2 V- Cthe washings in the volumetric flask containing the initial extract.
' O& M/ A h) {; Z# nRepeat the entire washing process two more times. Finally, wash the' U0 u2 }$ a" H9 Z6 |1 ^2 O4 r
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask3 v6 B' A5 C1 k$ M
to room temperature, dilute to volume with water, and mix.; |2 P( m4 ~! N4 p
Determine antimony, cadmium, and lead using an AAS/ICP-AES; Q: w5 d8 j+ G H; [; f
technique appropriate to the specified level. Determine arsenic using the* w8 k6 [3 R7 q) M e
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
$ M, K- J- [% VMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than% h8 `1 q. O! o; s E) r1 j, i
1 g. The selection of sample size and method of sample preparation) {% ]5 z( z% j/ V
may be based on the principles of the methods described in Volume 4.
: _' z# v2 ?) j6 g2 KAluminium oxide Reagents and sample solutions
* q+ i+ }( ?: l9 _1 E5 Q0.01 N Zinc Sulfate0 l( S' M, j: w/ @8 n& N4 G, x
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
0 C4 I. e6 H3 `: u4 hmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg8 S" L% V: G% W+ V2 k0 D
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of) `4 }; ^) e- G- Q) u
concentrated hydrochloric acid, heating gently to effect solution, then
3 C- A o+ Z5 n% U7 L$ ltransfer the solution into a 1000-ml volumetric flask, dilute to volume7 ~9 D3 s0 I" v
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500 g. s8 ?. \& h
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
, | M+ o$ C6 q7 Yconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
" G" [" j* h- E) c, y25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
! {% q; q. y8 {4 ddropwise, ammonia solution (1 in 5) until the colour is just completely
8 U" B6 k; M! O. ~" t6 |changed from red to orange-yellow. Then, add:
. m$ _0 e0 n' Q(a): 10 ml of ammonium acetate buffer solution (77 g of
, H% b% D6 l" i0 ]. yammonium acetate plus 10 ml of glacial acetic acid, dilute to
6 D3 f* L5 @0 L1 r0 | k& l, Z1000 ml with water) and! g- @! \; J7 I1 G2 |. [
(b): 10 ml of diammonium hydrogen phosphate solution (150 g3 H) ]$ Q4 e4 [& {: }! K; A/ [
of diammonium hydrogen phosphate in 700 ml of water,
5 e5 [8 u8 Q* n% H, Cadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,: D$ ^& X$ E4 n- U5 {
then dilute to 1000 ml with water).
% S8 F. k8 Y; r+ J# {/ v& K' aBoil the solution for 5 min, cool it quickly to room temperature in a8 p" _8 G: n. c1 p8 L5 d4 A
stream of running water, add 3 drops of xylenol orange TS, and mix.- y4 }1 R6 ~5 f! b0 s$ T% h
Using the zinc sulfate solution as titrant, titrate the solution to the first
3 C6 K$ r/ e$ f/ p+ n$ Uyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:6 B0 Q" z h, t3 u% Z- G
This titration should be performed quickly near the end-point by3 {- G5 @& O s r; U
adding rapidly 0.2 ml increments of the titrant until the first colour
% e! q8 M3 L% M1 U6 ^change occurs; although the colour will fade in 5-10 sec, it is the true
& W4 A% ?+ h- l" c1 {' S! Kend-point. Failure to observe the first colour change will result in an" j2 o2 E1 r/ c8 H
incorrect titration. The fading end-point does not occur at the second9 C" H3 Y: H. A$ @8 W A! J
end-point.)
4 P* w8 h6 b( zAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
* u5 ?9 ^9 ^4 b# P' Wstream of running water. Titrate this solution, using the zinc sulfate" a( G% `, ?5 U D+ N
solution as titrant, to the same fugitive yellow-brown or pink end-point; I6 g5 u$ T( b7 _. u8 T7 P
as described above.6 g& h. x% B" W" I, @% Q L- B3 @
Calculate the titre T of zinc sulfate solution by the formula:8 o, n, L# ?8 @7 @4 k! {
T = 18.896 W / V
+ g% F/ S2 G- K; kwhere! i' G- a# X. w9 U
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
3 H0 T( F: y' H% G. }W is the mass (g) of aluminium wire
' I6 x4 o3 i& D zV is the ml of the zinc sulfate solution consumed in the
: ?1 h, y$ d J4 ~% z1 \$ T* Nsecond titration4 ?% C0 ~( ^# i$ J4 W% M/ _- q
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and( `& h2 e8 v6 Y3 R2 U0 s/ @
R is the ratio of the formula weight of aluminium oxide to# j! ^) |* |4 G! j+ d
that of elemental aluminium.
0 y3 N0 ~/ M! W4 t9 h, j1 }Sample Solution A( e7 |: Q3 P4 M" q9 @
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica7 ^- Y9 E4 c; y4 e3 ]0 S6 t) N5 A
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).3 V/ u* h! n- _; D
(Note: Do not use more sodium bisulfate than specified, as an excess5 J1 y! c8 y' i$ n/ X; O
concentration of salt will interfere with the EDTA titration later on in the
* w) } ? i1 ]- Q4 r0 Qprocedure.) Begin heating the flask at low heat on a hot plate, and H2 Y# v1 M7 y" R/ h3 _
then gradually raise the temperature until full heat is reached.
" L: U, S' f/ s$ s; g(Caution: perform this procedure in a well ventilated area. ) When
$ \" v7 k9 k8 T# q n( uspattering has stopped and light fumes of SO3 appear, heat in the full
+ d3 j; C2 G1 _ ~4 qflame of a Meeker burner, with the flask tilted so that the fusion of the; _$ v5 u) Y, ^: f5 B1 R: D6 O( l, x
sample and sodium bisulfate is concentrated at one end of the flask.0 {3 j V q/ J, I9 I, @% a; {
Swirl constantly until the melt is clear (except for silica content), but
9 F% }1 h _% f: Yguard against prolonged heating to avoid precipitation of titanium
2 ~+ J: N! Y2 R- Fdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
) y4 u9 Z4 @% t. O" ~; m% lthe mass has dissolved and a clear solution results. Cool, and dilute to" U# Z4 b# I1 |, d6 Y+ f
120 ml with water. Introduce a magnetic stir bar into the flask.
: E4 _, Q2 E- [6 k0 hSample Solution B
0 K6 {/ k7 J( H n8 zPrepare 200 ml of an approximately 6.25 M solution of sodium
* i, N- W& ]2 T+ R* k4 |, ghydroxide. Add 65 ml of this solution to Sample Solution A, while# A; G3 n& L _% Z6 z& |5 I; k
stirring with the magnetic stirrer; pour the remaining 135 ml of the% ~0 L6 V+ {; T0 j* y7 ^! d# k. O8 ]
alkali solution into a 500-ml volumetric flask.; A! W* }. m9 p3 k9 t4 w% A: r
Slowly, with constant stirring, add the sample mixture to the alkali
$ H) `5 T) p# a, S0 {solution in the 500-ml volumetric flask; dilute to volume with water,
/ j. j# p$ R, g' H7 h* C( _0 u, ?and mix. (Note: If the procedure is delayed at this point for more than
4 e! j3 {7 w. S1 C8 j: l+ @) I: @2 hours, store the contents of the volumetric flask in a polyethylene. W& i& H4 u0 s) a% |
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
' {& c8 x5 [9 G' }# X& ^) Qthen filter the supernatant liquid through a very fine filter paper. Label
: D g" b6 f7 ]9 [) Bthe filtrate Sample Solution B.
, q% X; r$ r/ c+ P( oSample Solution C* [* V; A3 Q6 Q; \6 ^
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer2 v1 {9 Q( w+ s3 U
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid/ M9 j6 s: {( j/ a: D
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
5 R* P+ h3 W2 F. [# {M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is% p8 a5 O" y' [( L. Z
known, calculate the optimum volume of EDTA solution to be added
$ b) v5 e: s. o& n( Oby the formula: (4 x % Al2O3) + 5.]3 x% P6 n2 `3 x) {% x- u
Add, dropwise, ammonia solution (1 in 5) until the colour is just/ J9 q0 o6 H0 S, _: ]
completely changed from red to orange-yellow. Then add10 ml each6 D# R" j8 e, d
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to/ C8 [- I% _2 y9 F0 Z3 ?2 H
room temperature in a stream of running water, add 3 drops of xylenol" ~# b9 O( ?5 c# H" A O
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
+ U. u% j& _6 C) |5 ~bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
2 | [9 ^) A& N- q; e; u, A! ]pH, a pink colour indicates that not enough of the EDTA solution has
0 O# D4 h4 H& m8 [been added, in which case, discard the solution and repeat this
$ ^; }( S& @) ^$ ~/ Cprocedure with another 100 ml of Sample Solution B, using 50 ml,; X7 j3 D$ u! p+ M* N
rather than 25 ml, of 0.02 M disodium EDTA.
) J. ^4 _0 `0 h; _/ I( kProcedure
2 r7 T. c4 _! Z: f/ y3 r+ a7 sUsing the standardized zinc sulfate solution as titrant, titrate Sample
1 c& e, q& C* i1 B- F0 A5 XSolution C to the first yellow-brown or pink end-point that persists for
( C4 F$ M `* E7 R9 S) Z5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first0 c" E, g+ r' D6 V
titration should require more than 8 ml of titrant, but for more accurate
- x/ W! R; h* S/ O: G" _work a titration of 10-15 ml is desirable.9 Z% I* f& ~$ ~2 j; p2 a
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
7 [9 J, |6 K; Imin, and cool in a stream of running water. Titrate this solution, using0 x7 f& K/ v d5 [0 L/ C
the standardized zinc sulfate solution as titrant, to the same fugitive
. v# d/ {( |0 }1 y0 a) W9 Y, Oyellow-brown or pink end-point as described above.
. r# E; }( u, kCalculation:8 r; b9 j* P& u( {
Calculate the percentage of aluminium oxide (Al2O3) in the sample
( t2 w9 k# X4 D7 m4 t( n6 Ctaken by the formula:; e7 u) u. T, U) \; @. x# E
% Al2O3 = 100 × (0.005VT)/S
* W1 W* l$ q- M8 z+ kwhere
7 r* T! V1 y, s0 K. q3 _V is the number of ml of 0.01 N zinc sulfate consumed in
) i& d: U9 {! ?6 d# V9 M3 l6 }$ Qthe second titration,2 X) Z8 H7 K" L5 S
T is the titre of the zinc sulfate solution,
4 b" f D0 E0 j" P& BS is the mass (g) of the sample taken, and
. @ @0 x5 I$ x* v9 K& ?0.005 = 500 ml / (1000mg/g × 100 ml).9 _3 V, d& W9 L# V9 _ x
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
! u6 P+ a- X* G% D( H, Z1 l, t2 r& gglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O)., ~1 I% s/ G# v6 x% W9 d
Heat gently over a Meeker burner, while swirling the flask, until# a: x* b4 H7 O7 ]
decomposition and fusion are complete and the melt is clear, except3 L% U7 N$ [# D& W' Z
for the silica content, and then cool. (Caution: Do not overheat the
# C- S% h: u1 s& A! z0 F$ Tcontents of the flask at the beginning, and heat cautiously during
% ~' h/ o4 f/ _ T3 S# p- o% u' h$ Dfusion to avoid spattering.) `) ~. l3 V& F1 l
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat0 J h3 _' `) t0 q" o) t9 e' T
carefully and slowly until the melt is dissolved. Cool, and carefully add3 f! V1 S- c i; P2 T5 ]
150 ml of water by pouring very small portions down the sides of the
0 p1 ?1 E, r3 y' A: @+ M3 wflask, with frequent swirling to avoid over-heating and spattering. Allow( \- p' Y5 s6 H+ s9 O, e! \
the contents of the flask to cool, and filter through fine ashless filter
% Z- K5 I. J6 y1 R$ d' ~paper, using a 60 degree gravity funnel. Rinse out all the silica from
) O7 {# p, ]; k( }the flask onto the filter paper with sulfuric acid solution (1 in 10).
V* m$ G6 h& KTransfer the filter paper and its contents into a platinum crucible, dry in! @; A$ p- H- [1 W) F
an oven at 1200, and heat the partly covered crucible over a Bunsen- _! u8 ?* ? z. K2 [5 h I
burner. To prevent flaming of the filter paper, first heat the cover from
7 C$ _5 q8 L3 J6 f6 ^' Xabove, and then the crucible from below.
1 h+ `) g1 l; o# q7 F, D( K; l2 x, jWhen the filter paper is consumed, transfer the crucible to a muffle
1 \* A) l8 o* Zfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and' f9 O5 W& s3 {+ c# _4 X
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
4 g. W3 D4 R/ G9 G+ [/ [; [. U4 Xhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first& X4 |# u! x( M1 B
on a low-heat hot plate (to remove the HF) and then over a Bunsen
8 P2 U! n: |* ?! Fburner (to remove the H2SO4). Take precautions to avoid spattering,! g- B, S/ v) c
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
: X) u+ [1 k8 udesiccator, and weigh again. Record the difference between the two
E4 p V( w9 Y0 F% F; K8 rweights as the content of SiO2 in the sample.
2 Z9 J; X0 K5 N5 j; Y- i2 \$ aMETHOD OF ASSAY
1 E) O' o% r; q. i4 sAccurately weigh about 150 mg of the sample, previously dried at 105o
4 S" t$ W4 b" {/ V7 Gfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
' y3 K: N1 ]0 |and shake until a homogeneous, milky suspension is obtained. Add 30
. m9 t- A8 s& b' D; X. cml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially. D# r5 c& ]: s
heat gently, then heat strongly until a clear solution is obtained. Cool,
( J0 e( C. {& G9 f/ v+ Tthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
7 x5 O0 i. o! }: ~acid, and stir. Add 3 g of aluminium metal, and immediately insert a; A; A2 c7 }+ Y
rubber stopper fitted with a U-shaped glass tube while immersing the
: b" L9 Z$ L, Q% Q% h9 A3 zother end of the U-tube into a saturated solution of sodium
) A% I: r) M' b$ T* ]( i1 U0 ?% Qbicarbonate contained in a 500-ml wide-mouth bottle, and generate
5 M3 Z7 E' h! I- S- ghydrogen. Allow to stand for a few minutes after the aluminium metal0 ?0 P) k! Z6 I# Y- J
has dissolved completely to produce a transparent purple solution.
8 ?) ?# _/ F; I/ FCool to below 50o in running water, and remove the rubber stopper
7 r$ M$ i5 a! J: @0 E% s. q5 xcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate9 h1 \. \: q$ L! N
solution as an indicator, and immediately titrate with 0.2 N ferric
: w2 l# w0 S& C2 wammonium sulfate until a faint brown colour that persists for 30' L3 ^( O$ A6 V
seconds is obtained. Perform a blank determination and make any
7 R! @$ R4 u9 n1 `6 Xnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
; | s6 p+ U6 d" c/ ^5 [( D4 gequivalent to 7.990 mg of TiO2.
& P4 u& b& Q, m; _ r. _ T6 F |
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