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二氧化钛(钛白粉)
二氧化钛(钛白粉)) ^) r& l' b8 q: G ~$ C# ?4 B$ M
' ^, {- m. F3 @
JECFA关于二氧化钛(钛白粉)的结论
! H3 l, |- g: Y; ]8 N* ~1 U D+ ?* ~
摘要: 2006年JECFA关于二氧化钛的结论
" }* r. y" O" @& ]) U- X3 @$ i$ aADI值:不作限制。& F E3 f0 O W5 Y6 i& ~5 r# @
功能:着色剂
& ^7 e" q2 R! U2 `" s- B
% v% L: M, c: D- NTITANIUM DIOXIDE/ w8 A+ h5 v% _; w
Prepared at the 67th JECFA (2006) and published in FAO JECFA, o4 Z3 ]& ^$ b( g
Monographs 3 (2006), superseding specifications prepared at the 63rd
" H, q. n4 w1 ~, N7 r* BJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
6 {1 o; N: B& a* f' \1 X- mCombined Compendium of Food Additive Specifications, FAO JECFA) _' \" r- y0 e0 K5 y( }6 C: O% b
Monographs 1 (2005). An ADI “not limited” was established at the 13th, l+ j$ ~- S }- w
JECFA (1969).
1 Y) G% ?$ n# a# s$ tSYNONYMS5 H. y* \; l* b9 M: B) J
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
5 G. r N! Q- _) h, w9 a0 PDEFINITION
+ H' @0 j/ L1 |$ DTitanium dioxide is produced by either the sulfate or the chloride
' \/ y$ ?+ d. t0 kprocess. Processing conditions determine the form (anatase or rutile
8 ^ U) V3 u* t8 c! Gstructure) of the final product.& ?6 `7 `% B+ W/ ^ a% j
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
0 Z- ^, B' g( Eor ilmenite and titanium slag. After a series of purification steps, the# q$ M& ]2 a4 g- @( n/ I
isolated titanium dioxide is finally washed with water, calcined, and0 ^' r, R. U" ~0 n9 }
micronized.% C1 H/ F- H+ V
In the chloride process, chlorine gas is reacted with a titaniumcontaining
4 ~. J A' n. ~# T) }mineral under reducing conditions to form anhydrous
0 M) O+ k* A1 U6 N/ c# ]( M6 ltitanium tetrachloride, which is subsequently purified and converted to0 q3 s: B3 ~% l% g6 ]5 p5 i( z8 C
titanium dioxide either by direct thermal oxidation or by reaction with& m/ b* ^8 f4 x' ]7 c% _% k
steam in the vapour phase. Alternatively, concentrated hydrochloric# _/ k1 d$ v; G3 p2 Q5 e
acid can be reacted with the titanium-containing mineral to form a. e. a" w3 ~! ?: V- ]- l/ w
solution of titanium tetrachloride, which is then further purified and
+ ~# R" U+ W1 |; \converted to titanium dioxide by hydrolysis. The titanium dioxide is6 r) `+ e% e* e0 y2 ]
filtered, washed, and calcined.
5 @7 n) _. o2 C2 p4 TCommercial titanium dioxide may be coated with small amounts of
" H! q' K$ B; \1 G, F) _; c5 halumina and/or silica to improve the technological properties of the* _% h6 n1 ~7 G# ^2 B6 G- M
product./ t2 J% j7 K2 c8 |7 z
C.A.S. number 13463-67-7
9 @7 F5 J, ^( a* T# y( E FChemical formula TiO2
+ {* m& H* h) D( u7 f7 cFormula weight
! t7 \" q! a$ f3 }- s5 ?! G! C79.88) a7 _4 V& |1 g* {0 z) X/ v
Assay
% m- N# M _) f- G7 K2 `4 DNot less than 99.0% on the dried basis (on an aluminium oxide and M) [# U& {3 k
silicon dioxide-free basis)
4 n! Z; }4 Z( H5 tDESCRIPTION% `% F6 j- o4 {* Q9 a. V4 h
White to slightly coloured powder8 j t' i8 A; o
FUNCTIONAL USES( K: o1 g8 u, `% i
Colour
1 U, x v" v& V: Y% lCHARACTERISTICS
5 P& q& @: V) P( vIDENTIFICATION
+ K/ T$ E) l, N: q( ~5 g. |0 w' C& ]Solubility (Vol. 4)
. M" [* L1 f& d$ QInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
7 e4 T$ K* [8 v6 { m0 usolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
7 r6 p1 O6 q, k* Dsulfuric acid.0 D: |8 N& h# I }3 x5 j0 A
Colour reaction
" @' U7 Z, S% v) s# cAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
, w# X1 r1 |8 I$ t4 O1 Asulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
; |: D& \# ^* l3 f+ s: i& W/ `water and filter. To 5 ml of this clear filtrate, add a few drops of
6 M% x# Y8 F- jhydrogen peroxide; an orange-red colour appears immediately.
! W0 h0 z4 }0 [6 |* A7 TPURITY+ W1 t; E( ~# B
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
- J+ ^/ v! i$ @" _9 BLoss on ignition (Vol. 4). O* \* G5 n! e2 p% U7 ~7 p. a
Not more than 1.0% (800o) on the dried basis
. b. S& q0 s+ ?( y# I SAluminium oxide and/or
# o; l) C9 T( D. [* v4 Csilicon dioxide- B8 J% a$ R& ?* P6 C+ x
Not more than 2%, either singly or combined7 m* Z3 S7 j& m- N" I Q f6 h
See descriptions under TESTS
0 J. K$ r9 Y" o( x# n( w5 K8 bAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing3 r5 E/ c+ q0 Q2 ~& p( O9 I5 \0 O
alumina or silica.
9 Q) I( T/ K! S! fSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and4 R' i8 o! r% ]+ z1 y0 P) a
place on a steam bath for 30 min with occasional stirring. Filter
3 U8 p0 Z/ Z; J8 Wthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
& Q- B" a( x iwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
7 ]% a! m4 X5 I2 Q) mcombined filtrate and washings to dryness, and ignite at a dull red
8 E% X3 S/ q8 K' G( X6 e/ wheat to constant weight.
% Y" L* x6 v; E6 `8 r/ ~4 N" yWater-soluble matter0 N6 t7 |4 U' a; R
(Vol. 4)/ {, {4 ^& h9 ~# }+ Y& W
Not more than 0.5%3 ^5 v8 K# x9 ^* k+ [$ Z
Proceed as directed under acid-soluble substances (above), using8 ~- Q, y- o: {& Q5 V- F# _2 a
water in place of 0.5 N hydrochloric acid.
7 ~+ Q3 w# R5 a* E) ` `Impurities soluble in 0.5 N
" X+ z! X) }/ d% C" z4 Bhydrochloric acid# I" i2 i- z. \3 W
Antimony Not more than 2 mg/kg
8 B4 \- W& C: Q* R1 _0 B# s6 s, wSee description under TESTS
. Z4 N; d+ T- g6 ~: n2 Q; DArsenic Not more than 1 mg/kg, ?9 k) R& b N7 \6 r
See description under TESTS
& r# e+ y& `6 `6 ICadmium Not more than 1 mg/kg
9 b7 p0 h- R& }( P4 GSee description under TESTS
5 @- ~% W8 u! i, [% e5 \Lead/ A# B, o: k6 k* _" v) e S
Not more than 10 mg/kg7 H) N6 R; p3 v- A
See description under TESTS
1 @! R: p8 Q- @) T4 qMercury (Vol. 4) Not more than 1 mg/kg
; Y; ?0 O8 S L0 Y" SDetermine using the cold vapour atomic absorption technique. Select a- F- i3 u1 q% G9 ^
sample size appropriate to the specified level
8 o; ] y8 j& g3 WTESTS) s( \# I* k) C# ?. s
PURITY TESTS; [4 E( A: g( \7 q
Impurities soluble in 0.5 N0 M# E3 G; e" {, l9 L; Y' D
hydrochloric acid! R6 j+ ]3 r7 a' I
Antimony, arsenic,1 ~ C2 _/ Y% \* H
cadmium and lead% Z! g3 F, L* R: A/ {; p
(Vol.4)
- m+ J7 z K4 H* x- ~8 N2 Q1 wTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
2 A; X$ H5 G# v; {- g+ o: Rhydrochloric acid, cover with a watch glass, and heat to boiling on a
. H7 j. U2 Q9 V$ W* ?; P/ rhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml+ l) G! X4 ^* }& O/ y
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved3 M, R) I5 E" z0 W- E+ H
material settles. Decant the supernatant extract through a Whatman
, e9 V7 b9 k3 _' fNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
* v4 m* u& B$ avolumetric flask and retaining as much as possible of the undissolved
1 r7 ~2 J0 h) l; ~; a; G' tmaterial in the centrifuge bottle. Add 10 ml of hot water to the original D M+ e8 q H% k" q
beaker, washing off the watch glass with the water, and pour the
; y/ F7 q0 x% y6 q% p& y2 econtents into the centrifuge bottle. Form a slurry, using a glass stirring( x. H! O* A: F4 W2 w" R) K/ i
rod, and centrifuge. Decant through the same filter paper, and collect
5 x- T+ Q2 n6 c. k5 Qthe washings in the volumetric flask containing the initial extract.
3 F9 ?2 W; _7 mRepeat the entire washing process two more times. Finally, wash the) X; H# p8 }9 K: W/ _" r' j
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
: H/ g4 B: F6 W" H+ C5 u7 oto room temperature, dilute to volume with water, and mix.6 { O" ~; E+ W
Determine antimony, cadmium, and lead using an AAS/ICP-AES
( V" n9 ~# Z. Atechnique appropriate to the specified level. Determine arsenic using the6 W, ^" ]$ t+ d+ z- C' O7 e
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using! `4 `- \7 z( W6 V9 H/ F% y
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
* C% F F1 }$ o- j$ r! ]) S; ~1 g. The selection of sample size and method of sample preparation& L! k/ i% |% }. G5 ^/ {" p1 [
may be based on the principles of the methods described in Volume 4.
( D$ v6 C% P1 e& J! hAluminium oxide Reagents and sample solutions
# N7 W. u* I4 K0.01 N Zinc Sulfate1 j+ K8 G( s3 @
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
S5 k [6 Q) ~make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
* B& k9 j0 s6 y, Y1 q s( lof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of0 H) m$ i) b7 r: _
concentrated hydrochloric acid, heating gently to effect solution, then- Q3 {# P6 k2 U1 [
transfer the solution into a 1000-ml volumetric flask, dilute to volume2 @) M# c7 s0 U8 i9 ]' u6 ^" g; H; X
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
8 t3 P0 c% k+ gml Erlenmeyer flask containing 90 ml of water and 3 ml of2 }3 w. S8 q* Y- M, y
concentrated hydrochloric acid, add 1 drop of methyl orange TS and) m; K: }) b+ G$ M- z! Y$ G/ J* _
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
! C, a- j' i* v* Gdropwise, ammonia solution (1 in 5) until the colour is just completely& d m2 ~* f- g& w
changed from red to orange-yellow. Then, add:3 c/ v7 q m( d- r2 J5 ]
(a): 10 ml of ammonium acetate buffer solution (77 g of
+ n8 C$ E. g" _2 A8 @$ ]ammonium acetate plus 10 ml of glacial acetic acid, dilute to8 f; t! r* V2 m3 k4 `8 H& J
1000 ml with water) and
9 T6 k. s# N- l! |1 R$ ?% q(b): 10 ml of diammonium hydrogen phosphate solution (150 g* s' Z, i0 f' S7 v" o I
of diammonium hydrogen phosphate in 700 ml of water,3 C: Y" X* j6 E9 i
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
# T, L/ e3 j- b+ b0 ?2 Y5 x4 s1 j8 Tthen dilute to 1000 ml with water).
1 W; \1 B9 {. k* H+ S) MBoil the solution for 5 min, cool it quickly to room temperature in a
: X' T, s5 b& r x) _* f2 \stream of running water, add 3 drops of xylenol orange TS, and mix.4 l( x: A% o! u
Using the zinc sulfate solution as titrant, titrate the solution to the first, |+ Q7 C: F. Z# I
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:& r6 @3 ~; O/ D8 h
This titration should be performed quickly near the end-point by% N/ K; J4 N+ x; \. ] x0 H
adding rapidly 0.2 ml increments of the titrant until the first colour% q' x/ }* m9 B" i, v5 i8 r
change occurs; although the colour will fade in 5-10 sec, it is the true
. v7 l: C7 U% dend-point. Failure to observe the first colour change will result in an5 k7 p% \9 G# |2 g
incorrect titration. The fading end-point does not occur at the second
7 H$ s7 d" T& \end-point.)
; v9 u1 H$ P' b3 b# U. t9 \5 |Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
, I* u2 C0 O4 l/ B$ Jstream of running water. Titrate this solution, using the zinc sulfate( ?' b1 a2 z ]( L8 H- v5 |- {. H
solution as titrant, to the same fugitive yellow-brown or pink end-point: }% m9 e( m3 _ h: ]& o+ M5 N) g, [
as described above.& k- A, l) a S" D7 u* H
Calculate the titre T of zinc sulfate solution by the formula:# ?1 n6 z- z$ j5 l1 ~
T = 18.896 W / V& J' U4 G; g2 T, m) r
where' S4 }; A. @' y* k( O& B
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
o5 u F% ~1 B0 l6 [W is the mass (g) of aluminium wire
0 N+ X" p" S; r7 g1 i$ j1 {- sV is the ml of the zinc sulfate solution consumed in the
n4 f& w$ M+ ]& z) |: Fsecond titration
) L1 P9 C5 l. }& E" N5 T18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
1 j" {& Z0 {/ @2 d9 |8 MR is the ratio of the formula weight of aluminium oxide to/ y# t# j9 }: W1 Y) d8 }
that of elemental aluminium.* f3 ~) d6 |' K
Sample Solution A/ W9 i' F* ?$ N4 O; l4 d
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica6 E( b* @* j; ?9 J. t# ^7 A5 V
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
7 E9 U$ M0 P$ J. L- _( ?8 x2 h(Note: Do not use more sodium bisulfate than specified, as an excess
" L0 J0 _( i0 B* nconcentration of salt will interfere with the EDTA titration later on in the) G8 _) e x1 J
procedure.) Begin heating the flask at low heat on a hot plate, and' p1 ^! a2 C6 K$ W8 T, T3 z8 n9 r
then gradually raise the temperature until full heat is reached.
! O" N' r8 X" q$ _/ `3 u9 L8 V0 f" o(Caution: perform this procedure in a well ventilated area. ) When7 r2 [: @/ i# g/ a/ ?
spattering has stopped and light fumes of SO3 appear, heat in the full
1 T) Z Y) O1 Xflame of a Meeker burner, with the flask tilted so that the fusion of the
# w1 H# W/ T$ ~* Zsample and sodium bisulfate is concentrated at one end of the flask.- h, @- D) q+ I
Swirl constantly until the melt is clear (except for silica content), but/ h8 d% ]; L& A2 u. k
guard against prolonged heating to avoid precipitation of titanium
6 ?5 Z' b, C0 Qdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until! N( T5 v/ L3 M% G. E: z' m
the mass has dissolved and a clear solution results. Cool, and dilute to, z6 e% {* y3 Y4 m- S$ b
120 ml with water. Introduce a magnetic stir bar into the flask.
: r% Z# Q# n8 s- A- P7 PSample Solution B# j4 @+ a( f5 S& Q
Prepare 200 ml of an approximately 6.25 M solution of sodium( h9 K$ c8 |, V8 b/ u( }7 o$ m* m
hydroxide. Add 65 ml of this solution to Sample Solution A, while
6 a1 j; S* D1 {, Mstirring with the magnetic stirrer; pour the remaining 135 ml of the0 s* R+ }' a; C$ P: v1 m
alkali solution into a 500-ml volumetric flask. E I& j. N+ o" O3 f) W9 W- ^
Slowly, with constant stirring, add the sample mixture to the alkali: C, |7 }7 _, Y" c! M! a
solution in the 500-ml volumetric flask; dilute to volume with water,
& a( |8 G% t0 r5 F+ U- t) U: l" Zand mix. (Note: If the procedure is delayed at this point for more than
; E! z4 i7 P3 A8 v5 z* E2 T& y2 hours, store the contents of the volumetric flask in a polyethylene0 X3 Q- e) t: `3 b. c+ P3 p1 @* a2 B* T
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
& q# Z0 o7 i8 J$ bthen filter the supernatant liquid through a very fine filter paper. Label- y. K# R9 b9 W% [3 N9 S9 r
the filtrate Sample Solution B.
& I- R7 N4 g0 sSample Solution C& y0 V, p2 Z& w4 n
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer, G) c% z9 l; L* c7 J
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
5 R% Y' l, h9 e/ G8 G1 h! s6 psolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
( `! _! L! W$ e8 g0 \6 i; } n1 fM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
+ }2 t. d; w, I4 hknown, calculate the optimum volume of EDTA solution to be added, u1 p, b- W4 c& W
by the formula: (4 x % Al2O3) + 5.]3 s6 a/ N2 T8 o) j
Add, dropwise, ammonia solution (1 in 5) until the colour is just
1 i. i$ ^$ }6 n5 [6 G. \4 lcompletely changed from red to orange-yellow. Then add10 ml each
) P1 ~/ u7 e4 S3 Nof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to5 _+ G1 Z2 [- n! T/ Y
room temperature in a stream of running water, add 3 drops of xylenol
4 q U' `& i& J9 K$ d/ x0 ?orange TS, and mix. If the solution is purple, yellow-brown, or pink,
- r5 c& J- F4 e" D. w2 t& nbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
5 q9 B; `; V, g' A4 f. OpH, a pink colour indicates that not enough of the EDTA solution has
3 a* g W7 w3 ?2 O, Nbeen added, in which case, discard the solution and repeat this1 B/ k) H. q; o3 I: a" Q
procedure with another 100 ml of Sample Solution B, using 50 ml,
; ?4 T# m! ^5 s* ~* `* j% d6 h; hrather than 25 ml, of 0.02 M disodium EDTA.1 b5 i% x/ s5 r2 W
Procedure
& K: O& X& y9 y! Z, b o5 sUsing the standardized zinc sulfate solution as titrant, titrate Sample
2 i( t/ m) `% Q) mSolution C to the first yellow-brown or pink end-point that persists for
( C( D2 _0 g7 Z' R- ]5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first# W, B& u4 j `, F5 u# P" \* S
titration should require more than 8 ml of titrant, but for more accurate
% L3 Y/ ~$ F H- k0 X k, awork a titration of 10-15 ml is desirable.1 Y0 T4 x3 W% [5 H7 X7 K
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
) C7 d0 }6 f! h$ Z2 Z/ c P% ~min, and cool in a stream of running water. Titrate this solution, using( Q9 N# T6 }6 A% }5 z2 Q1 \
the standardized zinc sulfate solution as titrant, to the same fugitive
- }$ t# u% A3 [( Y$ }yellow-brown or pink end-point as described above.
, C/ ?/ ^, E+ i% I$ v+ qCalculation:
- x0 V0 F$ f; {( `' _3 rCalculate the percentage of aluminium oxide (Al2O3) in the sample
, @; W; m, l/ a9 S8 ltaken by the formula:
% z/ ]/ Q" G* d1 j4 B9 T% Al2O3 = 100 × (0.005VT)/S8 E# i6 ^+ B- E) O: Y% W
where! g9 l2 O; W$ M4 N
V is the number of ml of 0.01 N zinc sulfate consumed in
( {9 j& G* J' C, K# Kthe second titration,& r0 C$ z/ U" h0 p& K; {( m
T is the titre of the zinc sulfate solution,' E: K; X1 u# E8 Y9 M" y1 I3 z
S is the mass (g) of the sample taken, and* S1 X3 N8 {1 Y
0.005 = 500 ml / (1000mg/g × 100 ml). ^& o1 L: T/ {4 w0 o+ [6 E
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
5 H- c6 u: V D4 n' @glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
6 M$ o# |6 R0 wHeat gently over a Meeker burner, while swirling the flask, until* E, [0 I: U# y1 ], d( C
decomposition and fusion are complete and the melt is clear, except$ l+ x; S1 m* M' r) F& B' e
for the silica content, and then cool. (Caution: Do not overheat the
# h. Z* V% v+ n0 |: Tcontents of the flask at the beginning, and heat cautiously during
* w7 B8 J9 b/ _" ?1 \fusion to avoid spattering.)
1 s* d4 j. B- B1 w2 `! N2 c& rTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
# i1 W9 ?) n% r1 E( [: Kcarefully and slowly until the melt is dissolved. Cool, and carefully add
. Q+ H& J8 P( P150 ml of water by pouring very small portions down the sides of the/ i7 H1 w; {4 b+ N( f" K! V( ~
flask, with frequent swirling to avoid over-heating and spattering. Allow+ v3 n+ z% h5 o. w2 C/ p
the contents of the flask to cool, and filter through fine ashless filter
; B5 E/ \ p Lpaper, using a 60 degree gravity funnel. Rinse out all the silica from3 }9 g9 d( G4 h' Y' ]
the flask onto the filter paper with sulfuric acid solution (1 in 10).
- }3 Z& G6 o. u& \, @: [6 y6 ?Transfer the filter paper and its contents into a platinum crucible, dry in$ Y% u( V1 J: f$ s q
an oven at 1200, and heat the partly covered crucible over a Bunsen6 u# I% I: \) Q. k( \: B0 P3 o
burner. To prevent flaming of the filter paper, first heat the cover from
( Z- ]# Z9 j. q9 J/ C, _$ C/ a nabove, and then the crucible from below.0 S+ j. e% e! `8 A9 t5 }
When the filter paper is consumed, transfer the crucible to a muffle
& {+ s# S8 M; Q- M0 kfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and5 G4 y, V* M1 H$ s u
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
, E" o9 e5 \6 Fhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first* k1 b; N/ ?+ V0 q9 _% ^0 X P
on a low-heat hot plate (to remove the HF) and then over a Bunsen7 X' n6 o) Y& O, d
burner (to remove the H2SO4). Take precautions to avoid spattering,2 j2 H$ N% l! X$ U3 D8 Q. a9 v
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
; x+ u* P1 l+ a) Idesiccator, and weigh again. Record the difference between the two
# l1 E6 S* ~1 Z. ^/ ?weights as the content of SiO2 in the sample.0 p* F4 u% J* S" `; v
METHOD OF ASSAY
3 S; g' O: j+ mAccurately weigh about 150 mg of the sample, previously dried at 105o
2 u, O% l8 o" s: J' ^, c, `. _for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
0 I7 N/ A4 d' E' o) i0 _7 Dand shake until a homogeneous, milky suspension is obtained. Add 30
; T" Z! b5 ]. j D0 Aml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
" b0 |; A" R; \4 Jheat gently, then heat strongly until a clear solution is obtained. Cool,
. F+ ~# P! T* `! p, [: o' A+ Rthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
2 i8 X0 ?2 y) x* \acid, and stir. Add 3 g of aluminium metal, and immediately insert a- g% ~; c' y/ e
rubber stopper fitted with a U-shaped glass tube while immersing the1 }0 a8 ^- u8 t- E" N8 s7 O: Q
other end of the U-tube into a saturated solution of sodium# y/ U; Y: i; Z( i B' U' ?; {
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
7 { z5 f1 P+ g1 Q% M0 K* A; G1 `hydrogen. Allow to stand for a few minutes after the aluminium metal
* I" S( j- s) b& O8 T& }& ]3 k* b% Uhas dissolved completely to produce a transparent purple solution.
" T1 Q" Q9 W" J& l6 PCool to below 50o in running water, and remove the rubber stopper
+ {- C. @1 K! R# A. Kcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate9 q5 x/ X: H' d& [2 {; B
solution as an indicator, and immediately titrate with 0.2 N ferric
2 i; X1 |) W; C! Kammonium sulfate until a faint brown colour that persists for 30& u5 R, Y" g3 `* @
seconds is obtained. Perform a blank determination and make any
/ J. N8 K) }+ T" e I( p. ^1 enecessary correction. Each ml of 0.2 N ferric ammonium sulfate is, b' c0 d. E/ `* w+ [9 q
equivalent to 7.990 mg of TiO2.2 Y2 s9 ~7 S. @- W9 {- {
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