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二氧化钛(钛白粉)
二氧化钛(钛白粉)3 R5 |+ t) h) G" N. n- ?2 p
' u) m( d- p' oJECFA关于二氧化钛(钛白粉)的结论
; A9 m4 m9 w) O2 T. }" f: U, Z& Y6 ~7 @
摘要: 2006年JECFA关于二氧化钛的结论. D5 W, p% }) O
ADI值:不作限制。
* g6 G: o/ l. r9 }2 V功能:着色剂
0 @ ^0 G/ j2 k( E; s/ s3 _. D
s& T, a# \8 Q" r9 M- XTITANIUM DIOXIDE
0 g, Y- m( {5 D0 e) Y/ K" tPrepared at the 67th JECFA (2006) and published in FAO JECFA
$ z2 e1 z0 A/ d7 oMonographs 3 (2006), superseding specifications prepared at the 63rd0 Y1 v8 ] m8 r, [' z
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
: ?6 {. d/ a. G/ X9 [Combined Compendium of Food Additive Specifications, FAO JECFA& s; A, S* b( Y, p5 s
Monographs 1 (2005). An ADI “not limited” was established at the 13th
) E7 M2 D" c+ Z1 }9 ]1 J2 Y$ s% d7 {JECFA (1969). }" n1 s* y, _! t r5 G- @
SYNONYMS- L6 I) q6 z0 L& m! b9 f; ~
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171+ H2 A6 o7 g" H) v( Q% C1 n
DEFINITION; s: @4 T F9 [$ x8 {2 e# P
Titanium dioxide is produced by either the sulfate or the chloride* W- f1 k& z7 ^" I
process. Processing conditions determine the form (anatase or rutile! v9 L+ |; q) c
structure) of the final product.8 S, f% M9 ~( H/ X | x5 J
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
/ x4 [6 O3 `+ T$ Ror ilmenite and titanium slag. After a series of purification steps, the2 K% T- P* J) R8 l
isolated titanium dioxide is finally washed with water, calcined, and4 x' ~- _( ]: I% |! q. Z7 O4 p
micronized.$ Y, f6 F& u& `1 H/ F
In the chloride process, chlorine gas is reacted with a titaniumcontaining4 o5 v" B: a/ B
mineral under reducing conditions to form anhydrous* b- ?7 b) T- u
titanium tetrachloride, which is subsequently purified and converted to H7 d+ o# g- C4 p& d
titanium dioxide either by direct thermal oxidation or by reaction with5 D* h) W" J5 @ P6 @
steam in the vapour phase. Alternatively, concentrated hydrochloric
( H+ n2 C1 L# @acid can be reacted with the titanium-containing mineral to form a) B$ E& V8 j, _ b
solution of titanium tetrachloride, which is then further purified and& m* U }% E3 x4 \+ s5 Z8 R5 P. A4 W
converted to titanium dioxide by hydrolysis. The titanium dioxide is. ]+ x/ B) Z- `. \
filtered, washed, and calcined.: F" N; T# q8 N1 B2 _9 f3 @5 d6 ~
Commercial titanium dioxide may be coated with small amounts of
' A& I$ L. v) J: C1 ^+ v3 P K5 @1 palumina and/or silica to improve the technological properties of the0 \1 K1 R# }6 F
product.
1 [" E9 N* y7 a( ZC.A.S. number 13463-67-7
4 E% E _- w3 ~Chemical formula TiO25 `0 {& @" z" C& q4 ^ h1 J) x
Formula weight. H5 t8 V3 z9 i; L" U" g, N
79.88
8 Q. Z0 N5 p z& |Assay
- m5 L6 g, j7 i w$ u9 W! e0 uNot less than 99.0% on the dried basis (on an aluminium oxide and0 D4 z9 y# W" G; {
silicon dioxide-free basis)7 r+ @5 C+ }2 b; }8 W- x
DESCRIPTION
+ V1 a. ~9 [& { SWhite to slightly coloured powder! M+ h- Q& \! h3 _2 {
FUNCTIONAL USES2 M+ d. Y* h6 |3 ]7 Q: Z: _1 o
Colour
; c4 ?; q/ A1 U; o" O% i# FCHARACTERISTICS1 `, c9 I) x( n8 a* e
IDENTIFICATION- E6 g" {* J. p4 H3 q' n
Solubility (Vol. 4)
6 E. Z }4 l* T, T; ]* y9 a9 [3 h8 }Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
% Y& z X5 ]( b& y" t! {! h. Isolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
. K5 o4 a3 ~& }# lsulfuric acid.
5 q2 d" L! o& F8 KColour reaction
. `& G7 g8 W" A1 Y! d/ mAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of. e* o# M. v8 }2 L9 M$ _
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
, ^% d. u5 q! C+ c0 Q3 v0 jwater and filter. To 5 ml of this clear filtrate, add a few drops of7 g% ~; f Q+ o6 x
hydrogen peroxide; an orange-red colour appears immediately.
m S' j& j2 K, y( qPURITY
/ \. S! j& j5 `- s3 ELoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
h6 m1 j! ^& t( c; n3 L MLoss on ignition (Vol. 4)
& l {. B5 T. t( _/ S) yNot more than 1.0% (800o) on the dried basis" A* n: e; P: i( k* M* g# H
Aluminium oxide and/or
2 x7 S( b4 \7 O' t( e0 W" A5 ?; I7 ssilicon dioxide
9 y. a/ x$ U M9 ` h* C2 RNot more than 2%, either singly or combined9 I; q6 E# `$ W$ {9 N
See descriptions under TESTS
2 {2 ]$ N" E$ t0 {! iAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
; [* }( W2 c- G, J3 R5 ~alumina or silica." Q& S! L% c1 J3 K" _9 u# w
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
7 q8 W' r0 n5 K- z) F2 |$ Wplace on a steam bath for 30 min with occasional stirring. Filter' u1 X9 X' m6 F5 C$ K% y4 e
through a Gooch crucible fitted with a glass fibre filter paper. Wash; S; I& Y+ o+ L: I9 f, M4 n1 P- X4 N
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
/ w4 a$ w3 W+ p+ L$ A4 ]combined filtrate and washings to dryness, and ignite at a dull red0 B# T- D6 q3 w# n9 z+ F
heat to constant weight.
/ k. O" B# @7 C8 F) b8 i6 RWater-soluble matter5 |1 k5 I: d7 N& L) ]
(Vol. 4)- Z$ K9 g0 f% B. C w
Not more than 0.5%6 |2 K ^$ J q4 S! \- D! f# |
Proceed as directed under acid-soluble substances (above), using# K$ Y4 a' g* \1 s
water in place of 0.5 N hydrochloric acid.
I' p, C1 G5 qImpurities soluble in 0.5 N
! K, K. @0 H9 B9 l" P8 zhydrochloric acid- R/ @* b& Z+ l
Antimony Not more than 2 mg/kg
' m/ g; f# r/ R% T3 nSee description under TESTS
4 j; V: D* k! k# W+ h& eArsenic Not more than 1 mg/kg9 R1 }) ~. N( T& ~5 Z0 b4 _
See description under TESTS
2 t5 t t0 h4 O8 n5 G8 iCadmium Not more than 1 mg/kg, ~8 s! N3 |+ u& \5 l7 e9 E/ E
See description under TESTS: u0 p0 N3 o1 X7 T; c8 O: a
Lead
- n3 {. n7 W+ ?, ?- X. z# |' ^Not more than 10 mg/kg4 r9 w. _/ H# h5 ~; w
See description under TESTS
2 j& B- Y! M2 h, [! {/ k. QMercury (Vol. 4) Not more than 1 mg/kg
) A- u2 ^2 K% qDetermine using the cold vapour atomic absorption technique. Select a
" Y- }4 m$ E! [6 ^$ D$ J. x5 osample size appropriate to the specified level
) P/ O- b5 R: \, a4 |TESTS+ l1 |) \: r+ n: ^7 [$ P0 L& ^9 r2 J
PURITY TESTS
# l) _0 h, y) n, A2 iImpurities soluble in 0.5 N0 e& O2 U- q" w- `. @: F+ K1 J
hydrochloric acid# v+ F9 _5 a! N# h/ j: @) n v3 K! h
Antimony, arsenic,
6 x7 v! A0 v, O$ d9 Vcadmium and lead3 \* T+ S/ u' \" I
(Vol.4) A& H: p) d6 O# Q7 O4 O) y/ U9 \1 G
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
" p" @3 |8 D: Y. F0 Z; o; chydrochloric acid, cover with a watch glass, and heat to boiling on a6 k- o- ]7 J3 Y' e6 Z+ V
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml% a, {- V. x; v" `/ w( G
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved _; A5 u$ [- Q, B1 S
material settles. Decant the supernatant extract through a Whatman1 z* f- ]" b# U9 l D' {/ V
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml: q5 d. r$ T+ g# k
volumetric flask and retaining as much as possible of the undissolved
4 I; Q- D8 U, j9 r3 V$ y( ?4 o3 Imaterial in the centrifuge bottle. Add 10 ml of hot water to the original
% h0 T7 d5 R4 a; Wbeaker, washing off the watch glass with the water, and pour the& D; ]4 w1 b' \8 y( u X
contents into the centrifuge bottle. Form a slurry, using a glass stirring
" c8 p+ C a6 k( f: m) \. _7 {rod, and centrifuge. Decant through the same filter paper, and collect
* O# {" H0 w, p: @4 sthe washings in the volumetric flask containing the initial extract.
2 L% ?, Z$ Z# U5 m P# qRepeat the entire washing process two more times. Finally, wash the
4 f9 {/ X: v( \$ Z6 v' Gfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
( v2 g, {8 v6 W1 t, f6 V% c [& v6 lto room temperature, dilute to volume with water, and mix.
% {7 d5 _4 Y0 J( X% jDetermine antimony, cadmium, and lead using an AAS/ICP-AES
4 S5 ^* U% j: ?- B1 Q/ utechnique appropriate to the specified level. Determine arsenic using the
" o- a# V0 J4 {1 |1 p; sICP-AES/AAS-hydride technique. Alternatively, determine arsenic using/ B+ \3 O1 G8 c5 e7 p3 Q( Y# _
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
! ]- [0 o: t6 c* y1 g. The selection of sample size and method of sample preparation/ e5 U% q+ F; F2 J# D
may be based on the principles of the methods described in Volume 4.
9 z7 |3 u9 Y1 Q8 M1 h, BAluminium oxide Reagents and sample solutions+ D3 z; N- N, y& S, J9 z, v1 i
0.01 N Zinc Sulfate
" ?2 P6 B8 ?+ @, u$ @Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
4 {3 H: I0 H( _7 B- jmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg% |& ?! P; {5 C6 y
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
6 s9 w& d; t9 d, W3 y: yconcentrated hydrochloric acid, heating gently to effect solution, then
$ `( H& h9 _% F# C9 U# Ltransfer the solution into a 1000-ml volumetric flask, dilute to volume' j2 e0 M: h5 A! W7 W9 {: K2 r
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
( K# Q( t1 j* K7 ~4 B' B2 \5 [ml Erlenmeyer flask containing 90 ml of water and 3 ml of
7 ?: {1 K. g+ ~! w, O. econcentrated hydrochloric acid, add 1 drop of methyl orange TS and
, n. x% }6 d7 b1 \$ E7 F. j0 Z% n25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,8 x1 d) E; M2 }. q- i
dropwise, ammonia solution (1 in 5) until the colour is just completely
, [1 l' j* Q; C3 q% U0 d+ Q4 l1 Jchanged from red to orange-yellow. Then, add:
; c6 w2 h: K; [$ o1 ~( j9 Y) c. T c(a): 10 ml of ammonium acetate buffer solution (77 g of
) h7 X/ w1 \: Q- z) Zammonium acetate plus 10 ml of glacial acetic acid, dilute to
/ l {6 w* X4 X7 P. ]1 {2 L% j1000 ml with water) and6 b/ M% t6 G8 P8 n. X
(b): 10 ml of diammonium hydrogen phosphate solution (150 g' S3 [( g: r: ?5 h2 ^. u& f7 r5 X; A
of diammonium hydrogen phosphate in 700 ml of water,0 P5 g+ ^ O) ^/ g3 B) m/ ]$ T
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,1 T: q1 X6 i0 X7 u5 ~8 u% ]
then dilute to 1000 ml with water).3 m+ i+ _& J& _* b' q
Boil the solution for 5 min, cool it quickly to room temperature in a
2 d2 o- u+ o" Z N3 xstream of running water, add 3 drops of xylenol orange TS, and mix.
' F* D, ~8 j* ` Q m. UUsing the zinc sulfate solution as titrant, titrate the solution to the first$ C" P- m; x# h4 f
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:) }% K4 y: Q& s$ y3 d
This titration should be performed quickly near the end-point by
( w7 t- f" m H( w" d# L( ladding rapidly 0.2 ml increments of the titrant until the first colour
" u8 U' Y9 x; k0 f* X; gchange occurs; although the colour will fade in 5-10 sec, it is the true
0 |- V1 g$ ^7 G: Send-point. Failure to observe the first colour change will result in an5 T! ^# k9 {+ \1 z- G; p- [0 b
incorrect titration. The fading end-point does not occur at the second0 |* o$ {2 j g& O
end-point.), @: X) F1 s# C5 y. F4 B7 F; ?: v
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
7 D4 j( O' k& x6 I1 d! nstream of running water. Titrate this solution, using the zinc sulfate- k [( S/ [: K
solution as titrant, to the same fugitive yellow-brown or pink end-point
9 b- j6 `& b. ]# t, T& i' ]' @: Tas described above.' Q" V7 t# A# R! N; Q. _
Calculate the titre T of zinc sulfate solution by the formula:
8 p: @# b! T7 g/ n- QT = 18.896 W / V) G, M) H" K) l; [7 I5 j, V
where% E/ F- C4 C, C3 K
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution) }3 b) u2 c7 ~2 b, {. j* I. Y
W is the mass (g) of aluminium wire
5 h! t4 @9 ~+ ?$ @6 SV is the ml of the zinc sulfate solution consumed in the
; S$ d9 c' d$ F) L# a) xsecond titration
* E$ u: ?: B7 p6 g6 I1 }* l; x1 b18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and4 z/ x) ]5 c/ J* v( {' z# w) ?
R is the ratio of the formula weight of aluminium oxide to# i. K/ K1 n. V, l
that of elemental aluminium.8 |" p: j8 Z/ t5 ?: U2 I5 G
Sample Solution A h( s. Y; A% l8 {, `& W% O7 k
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica/ O d- A8 K6 S+ Z" b
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
1 i5 u0 P( W! o5 h& ^2 ^(Note: Do not use more sodium bisulfate than specified, as an excess
# Z$ V) V% W# [) Q5 econcentration of salt will interfere with the EDTA titration later on in the
* U4 Q# W) A5 t" |procedure.) Begin heating the flask at low heat on a hot plate, and
( g' z! F& g9 Xthen gradually raise the temperature until full heat is reached.
0 G: C# [6 A1 j(Caution: perform this procedure in a well ventilated area. ) When# @- C* \) y4 F$ U2 E3 f
spattering has stopped and light fumes of SO3 appear, heat in the full! l2 G( M' Y8 y7 ~$ r( Z# r! Q
flame of a Meeker burner, with the flask tilted so that the fusion of the, a- H/ [8 A" s2 z: T& N" |- R! x
sample and sodium bisulfate is concentrated at one end of the flask.
# z4 y, C4 h, M8 l1 W DSwirl constantly until the melt is clear (except for silica content), but
" X3 X/ N& T2 s5 ^guard against prolonged heating to avoid precipitation of titanium# n4 I& V# a/ D6 s. s) x. ?
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until; x. U+ {( K& P4 }7 T9 N) H. p; n
the mass has dissolved and a clear solution results. Cool, and dilute to8 d/ `' ^( R3 U9 R8 L& s/ `( a& i
120 ml with water. Introduce a magnetic stir bar into the flask.$ ?: q% V, e( _ c! ~2 }
Sample Solution B4 E* w5 J% G' |
Prepare 200 ml of an approximately 6.25 M solution of sodium- K0 r1 E! _1 q/ S g/ X, \9 l
hydroxide. Add 65 ml of this solution to Sample Solution A, while3 B& D2 w3 C' x! W7 W- v3 z, U( Q
stirring with the magnetic stirrer; pour the remaining 135 ml of the/ x3 D! J% s/ O: M3 p
alkali solution into a 500-ml volumetric flask.2 n- S! j: D, j2 n1 |! A4 f, h* n9 v
Slowly, with constant stirring, add the sample mixture to the alkali
G3 f1 P) B+ k2 t! T2 E& p' Ysolution in the 500-ml volumetric flask; dilute to volume with water,
0 a# i. y. @. ~1 tand mix. (Note: If the procedure is delayed at this point for more than; k6 o$ z M( N2 F# M: N1 _8 D
2 hours, store the contents of the volumetric flask in a polyethylene$ \7 _. y/ l) F: V: V
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),+ u7 w. n6 |- |; j9 ~- v
then filter the supernatant liquid through a very fine filter paper. Label
; O% a; [$ M; `2 Hthe filtrate Sample Solution B.
7 i5 K' g/ Z% [- a8 qSample Solution C3 \- ^8 L- V' S, d
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer, v& m) \# J1 p; Q2 Z& ^: o4 F" Y
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
* Q& }7 u3 \2 v7 Hsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02; Y9 ^3 [/ y. h9 _: _9 j1 y5 T5 v
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
3 ~) T2 A; ]% \1 l, I8 R% ?known, calculate the optimum volume of EDTA solution to be added
+ N. M/ K* y0 l5 Y" i) O, |# [by the formula: (4 x % Al2O3) + 5.]! b* D; ~' |* m, g
Add, dropwise, ammonia solution (1 in 5) until the colour is just+ u7 j) U0 i! y) d' a
completely changed from red to orange-yellow. Then add10 ml each
8 O6 L1 y, U" eof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
8 W; L! T" m- Vroom temperature in a stream of running water, add 3 drops of xylenol0 J3 H2 h c$ C4 f) F
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
; @" p% ^( Y# p, d, C5 Y2 tbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired, d& k' M1 \( D& b; t4 H6 x
pH, a pink colour indicates that not enough of the EDTA solution has
% ^+ {3 _' J2 q% y( U$ Cbeen added, in which case, discard the solution and repeat this
9 V1 }9 b/ m) ?9 V) e! B. Pprocedure with another 100 ml of Sample Solution B, using 50 ml,
5 B* U0 o3 O# U! K- W4 _rather than 25 ml, of 0.02 M disodium EDTA.
, s! q. M3 R( ^. S/ @6 Z9 f' @Procedure% b0 d3 l; S. j
Using the standardized zinc sulfate solution as titrant, titrate Sample" n, ?( A+ n; v/ J( x% V- f0 A" l
Solution C to the first yellow-brown or pink end-point that persists for
& o! l8 A) D" g5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first8 N' `/ X4 d7 j3 q
titration should require more than 8 ml of titrant, but for more accurate
3 s9 c: \8 ]4 ]+ g( F/ G+ R8 r% qwork a titration of 10-15 ml is desirable.
* ?8 x% x3 K9 l9 jAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5& ?/ D% c: R; ^- _' g: u' x
min, and cool in a stream of running water. Titrate this solution, using
& }' Z/ s# ?6 O, R* ]0 I; hthe standardized zinc sulfate solution as titrant, to the same fugitive0 u( J& h2 R% ]* z/ x6 i
yellow-brown or pink end-point as described above.
) k% |# W# t! Y) B) l, QCalculation:
8 L Y9 |% U- MCalculate the percentage of aluminium oxide (Al2O3) in the sample* d' I7 Q# O7 h" j2 X8 J
taken by the formula:- ]; L/ M8 n% u; P: s! }4 A
% Al2O3 = 100 × (0.005VT)/S4 G/ F: T c% H8 t( X: ]: O
where* T+ S0 g- B6 R1 Z3 P" M
V is the number of ml of 0.01 N zinc sulfate consumed in
* I& s; {0 D! O; ~# Jthe second titration,
) |9 J+ K; U+ h( t* g. {T is the titre of the zinc sulfate solution,
$ j# F) t1 _) h! m. B* b# tS is the mass (g) of the sample taken, and2 U" ?- a- n5 C3 @2 A: O
0.005 = 500 ml / (1000mg/g × 100 ml)./ |& B x1 a, [' s- i
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
: L! ^: G/ Q1 y* E/ P8 Rglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).4 z6 P1 j& e0 R; Y( x
Heat gently over a Meeker burner, while swirling the flask, until! W- G5 F8 I* I3 f1 x# C/ _. t) i
decomposition and fusion are complete and the melt is clear, except
* Y% {$ T* h* W0 ?8 L$ A Sfor the silica content, and then cool. (Caution: Do not overheat the
. X$ W6 y' L& ~( _! P ~0 ?contents of the flask at the beginning, and heat cautiously during
f) V4 P& z2 x2 H! O Gfusion to avoid spattering.)
) G8 S* B2 B t6 ^1 Q# }To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat* n m- s$ D; S4 i; q+ y: `
carefully and slowly until the melt is dissolved. Cool, and carefully add7 _$ r7 w$ f( G& q( B6 M
150 ml of water by pouring very small portions down the sides of the
8 [: N6 k9 V+ r6 W6 _8 gflask, with frequent swirling to avoid over-heating and spattering. Allow
" u$ }; b' d; | Nthe contents of the flask to cool, and filter through fine ashless filter
4 E) z1 f$ W0 ~; ?. ~$ \5 i! Xpaper, using a 60 degree gravity funnel. Rinse out all the silica from6 L/ t# T; V. ?+ D z) @! _- Q
the flask onto the filter paper with sulfuric acid solution (1 in 10).
7 p- b# s/ F" M1 KTransfer the filter paper and its contents into a platinum crucible, dry in$ |; d$ @- g& b9 t& H( L
an oven at 1200, and heat the partly covered crucible over a Bunsen
8 o4 |+ O7 R' ~. Qburner. To prevent flaming of the filter paper, first heat the cover from
) f' I3 M6 Z2 V0 F! V: [* R( U1 ]above, and then the crucible from below.! s" k# `, A3 w! ^$ V4 o
When the filter paper is consumed, transfer the crucible to a muffle
. t- I2 |1 }. u) x% x( Y( M# Yfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
) e+ v) X3 n5 W1 W: Q1 W# Mweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
* J* c, ^; y% l+ b. phydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first& P3 N. R+ w( m/ `4 f
on a low-heat hot plate (to remove the HF) and then over a Bunsen
: Z* a" A! W0 |/ K' rburner (to remove the H2SO4). Take precautions to avoid spattering,
3 J( S2 m% k+ F- Hespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
$ n* c6 `" l$ f0 }* fdesiccator, and weigh again. Record the difference between the two
9 |+ D& k7 W I" Fweights as the content of SiO2 in the sample.
8 ^# d3 X" Y' Q' c, Q5 Y: eMETHOD OF ASSAY
* w: J% O/ C- T+ _# f0 YAccurately weigh about 150 mg of the sample, previously dried at 105o/ H9 {* n) j4 _ P! ]/ @. z @
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water* @( ~' o% Q& _9 }
and shake until a homogeneous, milky suspension is obtained. Add 30
G- L# q) M% y- mml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
: {5 }; N. P; y6 rheat gently, then heat strongly until a clear solution is obtained. Cool,3 ?" L9 F9 R# u/ Q
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
: h) M* w+ i' d! s3 e5 ~acid, and stir. Add 3 g of aluminium metal, and immediately insert a
* `0 y Y9 _) B/ x+ P3 Mrubber stopper fitted with a U-shaped glass tube while immersing the
# s$ f6 {0 H% }3 M( Tother end of the U-tube into a saturated solution of sodium
- b, L% v6 O4 z* G3 g& p- Hbicarbonate contained in a 500-ml wide-mouth bottle, and generate
" r2 k0 ~. K) b: i& X1 A6 thydrogen. Allow to stand for a few minutes after the aluminium metal
8 {" h0 Y1 v! |; W* }has dissolved completely to produce a transparent purple solution.
% W& {8 L( w- I+ Q. lCool to below 50o in running water, and remove the rubber stopper! p& O% q8 }4 ~/ n1 i
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate3 T) S, l6 t; ^& J4 V
solution as an indicator, and immediately titrate with 0.2 N ferric" ~! n/ D& d+ o; F2 g' U* X
ammonium sulfate until a faint brown colour that persists for 30
$ i# T7 o! C, I! c* p* ~( b% [; tseconds is obtained. Perform a blank determination and make any }& }) F+ j" v
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
; ^# n, R) w$ H" u3 F, {9 L+ ]+ nequivalent to 7.990 mg of TiO2.
5 L8 w- O: W( M' c- ?6 E4 X |
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