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二氧化钛(钛白粉)
二氧化钛(钛白粉)
1 V0 i, k! m# Z
& b2 Z! O. [6 m( C& q* SJECFA关于二氧化钛(钛白粉)的结论
+ g' h& Q8 O5 S5 c, R' _+ m7 S$ m( N; S2 a/ m. O8 V P
摘要: 2006年JECFA关于二氧化钛的结论
8 Z' H- q+ z! U- S! ~8 c# KADI值:不作限制。6 s! A9 x7 f/ f& I
功能:着色剂
& B r6 A, U* z {7 x" z0 A
# x5 w4 {" Q: B& H4 P2 Q2 nTITANIUM DIOXIDE+ g! O: _5 K6 ]. [; j0 l
Prepared at the 67th JECFA (2006) and published in FAO JECFA
- u/ P5 e2 }7 n$ ~Monographs 3 (2006), superseding specifications prepared at the 63rd
7 }% o8 p M3 b2 n% ZJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
' n+ H1 K0 ~* ^! C* NCombined Compendium of Food Additive Specifications, FAO JECFA
u8 E4 f$ f" R. |! KMonographs 1 (2005). An ADI “not limited” was established at the 13th
1 o9 ~3 F! T _+ L$ vJECFA (1969).
- y: G- R2 |3 E0 f: pSYNONYMS7 M( R+ p; ]7 Q5 q. f
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171' Z: x7 z: p( C
DEFINITION- I4 N$ ?2 t3 n# D4 c' V) K/ _5 K
Titanium dioxide is produced by either the sulfate or the chloride2 X6 @+ E x& F- ^2 N' u
process. Processing conditions determine the form (anatase or rutile
) }4 t& B4 n5 _% C, b: T# R+ estructure) of the final product.
6 Y: [( d( w9 |# bIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)1 M- b( h f; ?/ ]0 R5 D6 \
or ilmenite and titanium slag. After a series of purification steps, the8 z' ~0 s/ r }7 u+ H5 |: M
isolated titanium dioxide is finally washed with water, calcined, and
! G! [. }( _4 e* j3 Qmicronized.
R6 }& R& J3 Z9 v& yIn the chloride process, chlorine gas is reacted with a titaniumcontaining
1 a, M- [8 B. fmineral under reducing conditions to form anhydrous( _ a$ r. K9 R
titanium tetrachloride, which is subsequently purified and converted to, O5 {$ {% `$ X, t( Y
titanium dioxide either by direct thermal oxidation or by reaction with
3 O" \/ Y5 Z" _. r+ f. i4 U' Y3 `steam in the vapour phase. Alternatively, concentrated hydrochloric" h/ G) ~" g/ `6 Z
acid can be reacted with the titanium-containing mineral to form a P) n/ d* d$ w, v O& d4 @) ~% ?
solution of titanium tetrachloride, which is then further purified and
* O e# g, ?/ v6 E, T. O. rconverted to titanium dioxide by hydrolysis. The titanium dioxide is
8 | I Z" J+ }: a$ m" M! C( Ufiltered, washed, and calcined.
! L8 o/ i4 h! D8 ~Commercial titanium dioxide may be coated with small amounts of) N: L; k3 ^6 Y9 S0 w
alumina and/or silica to improve the technological properties of the. `8 S. C+ B9 z
product.
9 @. G+ |. K* ] ]9 u7 w2 V5 P. wC.A.S. number 13463-67-73 B+ k# K. y4 W" v$ ]
Chemical formula TiO20 J5 r. T) c0 V& d! H$ m. f+ s
Formula weight
1 K" v2 p, f3 a7 q* E79.88
, b: u/ O7 {( X5 G+ {# DAssay) h& }" |$ ~0 m( d: Q( k7 {
Not less than 99.0% on the dried basis (on an aluminium oxide and
/ c2 k5 P+ H* e6 d5 z4 r0 [: ssilicon dioxide-free basis)) I+ Q$ |5 ]; L7 D0 o" R
DESCRIPTION1 o" S1 A0 e* ~2 ~! m# i4 F. h7 a5 f+ R
White to slightly coloured powder0 H% w2 Y. E6 H' K" b
FUNCTIONAL USES
$ a/ r z! A$ NColour
" M2 Y$ P" L/ A" `5 vCHARACTERISTICS
& ?# R& g- _# e( d- I# C( G0 Z Y* @IDENTIFICATION
( w) L- _$ I2 V" G' w5 NSolubility (Vol. 4)
' I2 x" ]! N, \; V* tInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
: H: E/ K/ p! y" Q9 _/ t% ssolvents. Dissolves slowly in hydrofluoric acid and hot concentrated7 [+ M8 h0 i: X4 I
sulfuric acid.
" h! T) }* F+ }1 H* TColour reaction% v% T$ ]- ?' h: o5 t
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
! O- {5 \* B' A" R1 z0 P) Tsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
- B8 H# K, V4 H9 [- q7 d" h1 Bwater and filter. To 5 ml of this clear filtrate, add a few drops of
8 W1 E0 k6 p* h# Z0 i, whydrogen peroxide; an orange-red colour appears immediately.
X1 N; G7 [" S. l% u1 d& z! |PURITY
; t% |% S3 Z, I+ N1 o/ tLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
' T4 i& Y( t& G. q" P' i) Y% XLoss on ignition (Vol. 4)
6 j6 I4 p6 V* ONot more than 1.0% (800o) on the dried basis
$ ]7 A2 V9 h: O8 Q- P2 FAluminium oxide and/or- f5 Z- W7 H7 p
silicon dioxide
0 n# r/ M9 X7 m6 n- w3 Z& z+ xNot more than 2%, either singly or combined* |3 c( n5 x8 }6 m; m
See descriptions under TESTS4 o l( `& q& L8 f9 `+ v
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing* ]# V- T2 ^/ j2 c9 e
alumina or silica.
" u6 H) C' r' N4 w/ u1 GSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and2 N' h# z: d4 u! L, q* @" ?; p
place on a steam bath for 30 min with occasional stirring. Filter
: v1 U7 Y0 W" H# n8 \- v/ fthrough a Gooch crucible fitted with a glass fibre filter paper. Wash! h* b- C: {2 O. f! _% W( Y$ F
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the/ W g+ i6 S+ o& ?: T' M6 r
combined filtrate and washings to dryness, and ignite at a dull red
/ S7 i' ]3 s. y: _5 y- Mheat to constant weight.
* V/ T) [9 H5 E! N5 k7 ]Water-soluble matter8 O7 l! q. g+ g! g6 O4 M; b, b8 z
(Vol. 4); O4 R9 g i2 E3 G8 N7 @
Not more than 0.5%
1 a; t* t F. k: T( CProceed as directed under acid-soluble substances (above), using& D/ u6 W/ u7 _* v
water in place of 0.5 N hydrochloric acid.
- @ [) e+ w$ q2 @Impurities soluble in 0.5 N0 @) Q8 q# U7 [- A" q# e
hydrochloric acid
i& w- w0 L' e. VAntimony Not more than 2 mg/kg$ i+ D: M* t/ K( o7 N" L
See description under TESTS
' x% _, K' B* O, `- o/ v& f6 YArsenic Not more than 1 mg/kg/ ~- a- ?1 Q0 W# w" v/ H
See description under TESTS
2 i/ S# ?; }0 }0 U6 ], Y3 q& \8 XCadmium Not more than 1 mg/kg1 m* Q6 B9 U! ]! z; Y4 U
See description under TESTS3 u$ a" N4 b. ?
Lead
U) E- \4 z6 x& |Not more than 10 mg/kg# u( O) F3 g5 U# F }$ x
See description under TESTS
# U3 H' m( C& WMercury (Vol. 4) Not more than 1 mg/kg7 ?" g/ m2 Y; F: P2 {
Determine using the cold vapour atomic absorption technique. Select a
, E' R1 k% T/ Asample size appropriate to the specified level
8 @, |, ?, h8 ]- z' QTESTS
- ]% d5 W4 l8 e! p k; r0 W; h& yPURITY TESTS
! N- ^ ?4 p& KImpurities soluble in 0.5 N: ?+ Z* T0 v m2 C' L4 ?; L* ~
hydrochloric acid9 v. B6 W7 T5 m C; r
Antimony, arsenic,
/ t8 Z' S N# h- q5 @2 K; r6 [, }' Icadmium and lead. n: P3 ]! ?5 j
(Vol.4)
+ h4 \% S" p; M7 c, wTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
* O2 G6 { h- \2 C0 N3 Z: ahydrochloric acid, cover with a watch glass, and heat to boiling on a
' M' e. q; k' p2 F7 Phot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml! f3 ?. X$ S* Q8 B$ s$ r# g7 \
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
. c5 N$ w4 u3 m+ _material settles. Decant the supernatant extract through a Whatman
% ]+ G5 ^% ?# s& p: ]No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml; `. ^/ @5 B. U$ ]
volumetric flask and retaining as much as possible of the undissolved% c* }: k1 M& p& e2 T' b0 r
material in the centrifuge bottle. Add 10 ml of hot water to the original
# y: u+ k6 w9 }# Tbeaker, washing off the watch glass with the water, and pour the
7 c" r8 D9 K* xcontents into the centrifuge bottle. Form a slurry, using a glass stirring# ]8 N6 d. t3 c/ s0 K
rod, and centrifuge. Decant through the same filter paper, and collect
' N9 S: c) ]6 `2 N, P: ^2 y; \& Bthe washings in the volumetric flask containing the initial extract.' ?5 W7 c- n. Q
Repeat the entire washing process two more times. Finally, wash the! B" O5 k c' |
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask6 e. Y! ]; B- i1 X% d( h
to room temperature, dilute to volume with water, and mix.
o; E# E+ G4 C! Z5 PDetermine antimony, cadmium, and lead using an AAS/ICP-AES
8 Q2 o: Y' i$ \& h( P6 Ytechnique appropriate to the specified level. Determine arsenic using the2 H+ A" ^8 F" j# k3 J. ^
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using2 b" a; q" g" k
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
$ p$ N0 X, f/ v+ c) {3 ?1 g. The selection of sample size and method of sample preparation# t) R- q* S; g, \ G& a
may be based on the principles of the methods described in Volume 4.
% ?& c$ H. c1 HAluminium oxide Reagents and sample solutions. A! n$ N% @0 f/ q9 `, v0 T) r
0.01 N Zinc Sulfate
( ~+ f: T5 T/ e% VDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
7 }- m! [, [' X# ]make 1000 ml. Standardize the solution as follows: Dissolve 500 mg6 r. X# `5 `1 a3 T
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
, t$ G6 y, v( k4 u5 } k( \concentrated hydrochloric acid, heating gently to effect solution, then, p9 Q5 i& K4 [) ~. o
transfer the solution into a 1000-ml volumetric flask, dilute to volume r2 [; x( l/ a* \, t( V
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
6 c- z. b1 Y- D3 l+ B! F; E4 Mml Erlenmeyer flask containing 90 ml of water and 3 ml of6 r% m; N, Y" v0 m* c3 x
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
- u! _7 P; V4 e25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,; n1 Z8 m7 [3 R/ Y5 t0 W
dropwise, ammonia solution (1 in 5) until the colour is just completely" U2 T/ e$ b8 ^# u v2 m* z
changed from red to orange-yellow. Then, add:' M" Q/ R: @) \# ~2 W
(a): 10 ml of ammonium acetate buffer solution (77 g of" d* a3 {& f) A+ z5 `4 V1 |
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
" W/ V$ V! Q1 y7 m3 U1000 ml with water) and# j, a) K" `; w& a" D9 l: d7 U
(b): 10 ml of diammonium hydrogen phosphate solution (150 g* K4 e3 X4 Z9 `1 Z, M
of diammonium hydrogen phosphate in 700 ml of water,+ `7 }' I& D) \( N
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
- A3 Q5 v7 }; q. d: ~8 v4 ~5 ]$ `& A: s3 Qthen dilute to 1000 ml with water).9 B* F% ]* \, I
Boil the solution for 5 min, cool it quickly to room temperature in a4 q# N3 w+ Z; R" S
stream of running water, add 3 drops of xylenol orange TS, and mix.4 @: a& k& Y5 m4 W# N. {' G
Using the zinc sulfate solution as titrant, titrate the solution to the first
! P1 O5 Y; s. L4 q4 S" N3 p& iyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
% I3 y5 y/ Y, {: I7 U! ?* m6 |8 Y8 gThis titration should be performed quickly near the end-point by
$ R' S' a: w. G& b4 ^adding rapidly 0.2 ml increments of the titrant until the first colour3 ?: W8 y, l# D8 T3 g. Z+ |( ^* t
change occurs; although the colour will fade in 5-10 sec, it is the true
B* Q1 k& G$ @ J" dend-point. Failure to observe the first colour change will result in an
( U j2 E1 E4 E/ u5 z. z4 {incorrect titration. The fading end-point does not occur at the second
+ e! t' g; h6 ~* L' Rend-point.)+ V4 S* O- S+ a
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a4 m, K! ]* ?! ^7 o6 a0 ?
stream of running water. Titrate this solution, using the zinc sulfate
; h* ]" ~2 @: F% P+ c. N! Rsolution as titrant, to the same fugitive yellow-brown or pink end-point
j$ c" t2 i4 P$ o/ r& z9 Ias described above.
" i4 [0 Y* Y" u% p7 S UCalculate the titre T of zinc sulfate solution by the formula:
@- a0 ?* I, o- r$ A l* Z3 }T = 18.896 W / V. [3 }# i- F, V8 u/ }8 K
where5 W, C+ U K. J9 J0 L
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution" r/ s# t/ S8 w& K) ~5 N2 \3 k
W is the mass (g) of aluminium wire
% |- M8 T' t* A4 s( sV is the ml of the zinc sulfate solution consumed in the
7 L% v# a& G3 n! h: m8 Wsecond titration$ M% h k1 M/ |; t' G
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and0 P. Y: R% [ I
R is the ratio of the formula weight of aluminium oxide to, b* D# x6 d5 J$ v& T
that of elemental aluminium.' N7 `2 b5 }8 |1 X/ Q, L9 {: w
Sample Solution A, D+ a# y& t' g. Z" \
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica, f' c7 q4 C, t$ O
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
- C$ z% V' U' V" m8 L(Note: Do not use more sodium bisulfate than specified, as an excess
, i! d9 t3 q2 Aconcentration of salt will interfere with the EDTA titration later on in the
5 `8 U( B* f. b' R6 M1 Xprocedure.) Begin heating the flask at low heat on a hot plate, and
( S h0 d' {, X8 Mthen gradually raise the temperature until full heat is reached.
) I5 V& }4 g3 L6 a(Caution: perform this procedure in a well ventilated area. ) When: G1 y0 @, i2 c0 O4 L9 m6 ^- A& Z
spattering has stopped and light fumes of SO3 appear, heat in the full
4 g0 J5 k5 Z& z4 L/ Y$ W& Aflame of a Meeker burner, with the flask tilted so that the fusion of the& {- I2 S4 Y6 O, Y! o7 T+ D
sample and sodium bisulfate is concentrated at one end of the flask.; U" j- m) V9 P( l9 C
Swirl constantly until the melt is clear (except for silica content), but
& K. S! M. b' g v+ Eguard against prolonged heating to avoid precipitation of titanium
8 {' B9 E) F" F" E" Fdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
, q6 F( v9 g; l' d, y* rthe mass has dissolved and a clear solution results. Cool, and dilute to" ~) P& G" X) n6 K/ N. N+ a% c6 n
120 ml with water. Introduce a magnetic stir bar into the flask.# @9 r; s% @' j! q& b( g/ d
Sample Solution B
) H/ ^. Y4 Z9 n! Z' j3 x# I+ ^Prepare 200 ml of an approximately 6.25 M solution of sodium
$ E+ b$ w+ Z& b4 O" L& Z Ihydroxide. Add 65 ml of this solution to Sample Solution A, while
, S4 t% n7 n7 z$ X! y, @stirring with the magnetic stirrer; pour the remaining 135 ml of the
3 ~4 G* S- U! B8 K) c/ `- \alkali solution into a 500-ml volumetric flask.
0 ]4 s+ l5 u0 I9 ^% H, m# ?' Y3 OSlowly, with constant stirring, add the sample mixture to the alkali0 x5 e" Z9 M% j# a% }6 b. L) u
solution in the 500-ml volumetric flask; dilute to volume with water,
d1 k3 F4 c. g: c- _and mix. (Note: If the procedure is delayed at this point for more than. F/ j, z$ r( D& @
2 hours, store the contents of the volumetric flask in a polyethylene
* \* T+ V! n6 }bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),3 W$ E2 C; h, r1 j: V4 h% t
then filter the supernatant liquid through a very fine filter paper. Label
2 O& e, j5 O3 E+ Rthe filtrate Sample Solution B.
& D# h j, _ Q& \; lSample Solution C
: y. Q% l, _" [1 C* WTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer7 k! ]* K/ g- v2 Y( D# [
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid! p) q! T* g# O6 Q. s5 c( b
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
% }0 o. z7 ^' t6 B" MM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
2 Q# o* T1 B( w" o; O; ~0 ^known, calculate the optimum volume of EDTA solution to be added- l0 o) w9 ]3 p1 b m
by the formula: (4 x % Al2O3) + 5.]
: V! w. f8 m0 N3 B f% F4 OAdd, dropwise, ammonia solution (1 in 5) until the colour is just* F2 q- h: M1 q. z, ? j
completely changed from red to orange-yellow. Then add10 ml each! |, p5 E# v" a+ B5 X& q
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to+ x8 y6 ?2 i& q" y
room temperature in a stream of running water, add 3 drops of xylenol
- Z: U; e, O( M+ borange TS, and mix. If the solution is purple, yellow-brown, or pink,
: A5 R0 ~7 K. v6 `bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
- `! j8 H4 c) q6 P; ipH, a pink colour indicates that not enough of the EDTA solution has
_8 U0 E, [- D7 D! d' _2 _4 Ybeen added, in which case, discard the solution and repeat this! R- r. Z; O8 X1 q+ I, Y7 k x
procedure with another 100 ml of Sample Solution B, using 50 ml,
. d6 T6 j1 e- I' ^4 Hrather than 25 ml, of 0.02 M disodium EDTA.
8 H, p. a7 w2 v' g0 M! L- bProcedure
. r* X n5 P8 A4 b' ?- uUsing the standardized zinc sulfate solution as titrant, titrate Sample
, [. Q+ l! O5 h* }# F* V' \1 vSolution C to the first yellow-brown or pink end-point that persists for3 r" Z4 o: r/ L) G6 {1 o, }
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
$ y/ _3 [( j( C( i, w9 Ititration should require more than 8 ml of titrant, but for more accurate$ y# Q/ h: r5 S; A
work a titration of 10-15 ml is desirable.# c: t h% f0 I' Y
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-53 a1 B& `; w8 m7 Z- [
min, and cool in a stream of running water. Titrate this solution, using* |; {" a( N, P
the standardized zinc sulfate solution as titrant, to the same fugitive
# r" [! K# U7 P' p! J0 P% C) X7 ?0 Xyellow-brown or pink end-point as described above.
& r( b4 G) K' c! JCalculation:
* C2 c5 Q2 P5 _3 T N' @* S( F/ QCalculate the percentage of aluminium oxide (Al2O3) in the sample0 n. |# F/ y7 ?
taken by the formula:/ B/ Z1 E" }$ v" g; }4 S: ~
% Al2O3 = 100 × (0.005VT)/S: r. I2 O* d8 Z/ A0 |
where
, x- T3 x$ S6 aV is the number of ml of 0.01 N zinc sulfate consumed in7 ^. C) H. q8 B+ V$ W# P. J2 i
the second titration,/ O* R6 u! j* E# N# d5 P
T is the titre of the zinc sulfate solution, K0 X& f1 N' A% {: z! l
S is the mass (g) of the sample taken, and
0 F4 ~6 h8 n% g/ R2 \& @0.005 = 500 ml / (1000mg/g × 100 ml).+ p2 V: O q% r X: D+ Z u2 J
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica8 u, j* a; o" ^; u. l/ y
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).5 W0 M6 R1 P. S
Heat gently over a Meeker burner, while swirling the flask, until
/ R/ y" K$ o1 a/ |+ m/ |7 @% ddecomposition and fusion are complete and the melt is clear, except
7 R \2 {$ L7 ` ?3 _4 sfor the silica content, and then cool. (Caution: Do not overheat the+ S$ w, j) D( `' G. u/ l' O
contents of the flask at the beginning, and heat cautiously during- c2 h3 Q7 B4 j- r/ @( Y
fusion to avoid spattering.)% y) r5 I) F8 I8 y# C$ y; R
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
9 F( T. K2 f. \1 S0 tcarefully and slowly until the melt is dissolved. Cool, and carefully add
2 w8 q* y6 E+ ]3 d8 M1 k8 c: z150 ml of water by pouring very small portions down the sides of the j* z* l* B3 b/ ^
flask, with frequent swirling to avoid over-heating and spattering. Allow
4 M8 M$ e* H* O8 l4 b/ X& Gthe contents of the flask to cool, and filter through fine ashless filter
6 p0 u! v F; b9 I# M _9 m$ `paper, using a 60 degree gravity funnel. Rinse out all the silica from4 O* a9 l- X2 Y4 `: }
the flask onto the filter paper with sulfuric acid solution (1 in 10).) C! y7 I9 J# U9 r
Transfer the filter paper and its contents into a platinum crucible, dry in
! \6 `; c& t+ y. a7 t6 o. Uan oven at 1200, and heat the partly covered crucible over a Bunsen, q! l* H# M5 M) n0 p; A% a' y( C
burner. To prevent flaming of the filter paper, first heat the cover from3 v, y3 z- X& O2 [( Q- _
above, and then the crucible from below., ], M- `; @7 L: I) D
When the filter paper is consumed, transfer the crucible to a muffle& k4 s) e# @* \; N6 [ x
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and! p/ t6 y$ ^$ Y) a- O# q" D
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated% G3 ]5 J8 R0 i* o
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first' D& x- C& A: H9 F
on a low-heat hot plate (to remove the HF) and then over a Bunsen
( ]5 _1 g2 f: E: s7 y& R' Aburner (to remove the H2SO4). Take precautions to avoid spattering,
1 Z$ W$ v2 Q& S% q2 H/ k& [. nespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a$ r9 r7 E" O0 _8 |7 d2 ]" I# K
desiccator, and weigh again. Record the difference between the two/ u% R; Q- o5 I- @+ g% F
weights as the content of SiO2 in the sample.% c) V7 `# r1 `7 E6 S1 { z4 i
METHOD OF ASSAY
; m6 g5 |# e' a0 |' y/ KAccurately weigh about 150 mg of the sample, previously dried at 105o
% r8 c7 B3 Z& Cfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water6 L" H- `, r8 v$ E3 G: a) `6 ~
and shake until a homogeneous, milky suspension is obtained. Add 30
: ^ C5 `* T1 q/ ~5 s$ i" l8 D: ^" Sml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially% K# y: l9 v% }1 a7 l
heat gently, then heat strongly until a clear solution is obtained. Cool,
+ u D% y' R/ Q8 y1 L7 ithen cautiously dilute with 120 ml of water and 40 ml of hydrochloric2 V; i+ c& V" I% o- p6 G
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
$ ]! w0 K$ Z/ u7 Mrubber stopper fitted with a U-shaped glass tube while immersing the
/ V7 O& s6 M! U0 K& u; ]other end of the U-tube into a saturated solution of sodium
8 Y8 o( Z1 p8 t8 T3 x, Z6 }bicarbonate contained in a 500-ml wide-mouth bottle, and generate
4 x: u0 ^. x' }" P0 L+ shydrogen. Allow to stand for a few minutes after the aluminium metal; ^2 @, ?! p: r8 m: ?
has dissolved completely to produce a transparent purple solution.
0 O9 g5 a w7 G1 NCool to below 50o in running water, and remove the rubber stopper: O* S: L$ H& A- \
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate, u1 f Z- \! Y9 U
solution as an indicator, and immediately titrate with 0.2 N ferric
) F3 M4 `) ]3 p% C. e5 v, {ammonium sulfate until a faint brown colour that persists for 30
. V# j- d) k: t" sseconds is obtained. Perform a blank determination and make any
2 K! O. Y4 B2 C2 _necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
) S4 Y$ l$ `7 C6 A8 S! {equivalent to 7.990 mg of TiO2.9 W1 ~( Z" w/ x' ~7 S, W
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