|
沙发
楼主 |
发表于 2008-5-23 12:10:00
|
只看该作者
二氧化钛(钛白粉)
二氧化钛(钛白粉)
+ d F, U/ O4 \! Y4 r! L1 s0 J5 {
6 k, {* I: k- g% CJECFA关于二氧化钛(钛白粉)的结论4 z7 L' c v5 }/ V8 e0 R& S& ~
1 N5 J# h# U# H5 X, l, |) [$ `* e摘要: 2006年JECFA关于二氧化钛的结论
7 [/ F( Y- i2 s! VADI值:不作限制。
& N6 T, j- @7 l4 @& e# y功能:着色剂
/ `! `& u( {" z r* M4 h- K
& g. b: j4 a1 ?6 vTITANIUM DIOXIDE/ m0 m5 V: Q* O
Prepared at the 67th JECFA (2006) and published in FAO JECFA
' W9 a; l, T- z8 \Monographs 3 (2006), superseding specifications prepared at the 63rd6 D& t3 t6 S: j" ?" v# W
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
$ K; @$ h" g9 b x/ R' [Combined Compendium of Food Additive Specifications, FAO JECFA
' N$ w9 {+ s2 e9 a( ~Monographs 1 (2005). An ADI “not limited” was established at the 13th$ R* p: ~4 m6 U' L3 Q& ~
JECFA (1969).' R' Q7 r9 u* d- ?: Y$ L4 {
SYNONYMS5 a* E9 \, b% F+ D/ U
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
1 a- Z4 b& ^# K* kDEFINITION
' ~) S3 h( }" ^ V5 y1 HTitanium dioxide is produced by either the sulfate or the chloride
; _1 P# v3 V/ o* g P' z" Kprocess. Processing conditions determine the form (anatase or rutile8 U9 V& n( J) r1 V/ {2 O( _7 s
structure) of the final product.; O& R; E$ [" ]! r% C
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
$ J5 w0 W* E% Y. {" D. Oor ilmenite and titanium slag. After a series of purification steps, the
+ G% z1 `4 m) } X4 {" q& t" n( |8 }isolated titanium dioxide is finally washed with water, calcined, and- ?& |) H" f8 G
micronized.
3 ^2 `) u0 }1 MIn the chloride process, chlorine gas is reacted with a titaniumcontaining
: i/ U- [! p7 c |/ S7 Q! Ymineral under reducing conditions to form anhydrous. F3 i7 u' U; p! ~' c4 p2 h
titanium tetrachloride, which is subsequently purified and converted to
! ~, I* a' \& c7 I1 R# {titanium dioxide either by direct thermal oxidation or by reaction with
5 u" X% |! l) a: _, q+ Lsteam in the vapour phase. Alternatively, concentrated hydrochloric+ W0 d2 w; D$ E A; n" N5 l
acid can be reacted with the titanium-containing mineral to form a
, u/ l6 a+ U0 L" u3 M# M8 E$ Ysolution of titanium tetrachloride, which is then further purified and
9 \# e! Z- j/ f1 n+ K6 hconverted to titanium dioxide by hydrolysis. The titanium dioxide is& q* t' y1 C Q4 t$ {: Y) m8 f* Q, s
filtered, washed, and calcined. o$ r7 F, s2 {) H Z: v
Commercial titanium dioxide may be coated with small amounts of
" M% C6 H7 U2 L* j0 b. `* calumina and/or silica to improve the technological properties of the* O( l6 n# ]9 [2 n. u) _! h
product.
% ` j. B0 _. v3 B* y0 L( p$ |C.A.S. number 13463-67-71 ~7 U2 o: E& K
Chemical formula TiO2
4 Q9 G ]8 F1 ?) O* oFormula weight
, @, r7 @ c. N79.880 f0 o8 e" z9 ?$ m5 @/ D6 x' x
Assay1 I/ [* p) P0 X( ?& `
Not less than 99.0% on the dried basis (on an aluminium oxide and
- J3 {2 x6 z6 ^4 P1 y( osilicon dioxide-free basis)
( p; N5 M& `, W/ a( O0 PDESCRIPTION. C q- t8 ^, K5 L
White to slightly coloured powder
. f8 _) I0 R. J* LFUNCTIONAL USES
# |* Y$ ~3 V3 O+ DColour4 f) r1 P* I8 y2 L& x
CHARACTERISTICS- J1 L' c% s- x
IDENTIFICATION
b; i' N( A/ @# TSolubility (Vol. 4)
6 X4 t6 J4 `+ \( H& \# R/ _% eInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
1 }/ k @+ h5 t) E& F8 d; w/ u$ @solvents. Dissolves slowly in hydrofluoric acid and hot concentrated. b1 D2 B: o; G5 V" D. ^5 }
sulfuric acid.
/ a* I4 s; g0 `0 I1 {Colour reaction" ]& ^$ ^) l4 R" L9 Q. ^3 ^4 ~3 ]
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
& n; O6 G# D! l! w- X$ Xsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
8 _9 [5 }: j, Z( Ywater and filter. To 5 ml of this clear filtrate, add a few drops of
i. p J+ D) B' P+ Qhydrogen peroxide; an orange-red colour appears immediately.& J0 g5 b/ R$ I8 t, r; y* t+ E
PURITY
, b9 x2 g, w; Q; Q$ |/ iLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
: q/ ]4 @5 {) t5 l# K4 ^) fLoss on ignition (Vol. 4)7 L y# B U7 A3 _
Not more than 1.0% (800o) on the dried basis
- z0 R; w% }5 T6 n1 V8 N4 }Aluminium oxide and/or
8 Z8 D( w1 B. y# msilicon dioxide0 V% c% G! m# T; b/ V
Not more than 2%, either singly or combined
" S& s9 o# |: c+ WSee descriptions under TESTS) i2 @1 k; k& |$ M/ `
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
0 ~' R1 N0 p# L! N3 [5 aalumina or silica.# X6 _7 E- y5 x& B1 n" Z
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
: M* {) p& w: ]) e3 L m3 e; S* uplace on a steam bath for 30 min with occasional stirring. Filter
4 m) H5 I# @& g5 t' z- `8 F" othrough a Gooch crucible fitted with a glass fibre filter paper. Wash8 a* n T2 y6 _& c
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the, V' V% ]6 I1 M' D3 p
combined filtrate and washings to dryness, and ignite at a dull red0 J$ P6 x! w8 I+ H s$ s
heat to constant weight.
3 k9 J4 _* |! e9 ?, GWater-soluble matter1 L) A7 h- {. I/ C: o
(Vol. 4); Z2 T" V2 {8 P f' e7 ~
Not more than 0.5%
+ H; c/ c: n8 G' Z9 e+ PProceed as directed under acid-soluble substances (above), using
" Y5 D3 k) k4 B8 Z; Nwater in place of 0.5 N hydrochloric acid.
; J6 O9 H& d+ Q7 L7 L4 E0 h+ EImpurities soluble in 0.5 N
?( \; V3 n0 E, \' }hydrochloric acid
$ w2 _7 H0 I- ?1 n( d9 I [3 pAntimony Not more than 2 mg/kg
- y0 M# a) L9 u8 Z) ~2 OSee description under TESTS: B+ z7 ?; x% v1 m
Arsenic Not more than 1 mg/kg8 ~! X3 S+ H4 j' \3 C u
See description under TESTS {3 u6 I4 d% a; s+ o" D9 e
Cadmium Not more than 1 mg/kg
" B3 Q' d, Y7 ^See description under TESTS
6 x) |4 ^6 q. e% J! ~Lead3 P& E9 ]1 b- f: Z# o, V
Not more than 10 mg/kg
( ^9 C! ]' t SSee description under TESTS
4 q8 i- D6 `/ E* B9 vMercury (Vol. 4) Not more than 1 mg/kg
$ o9 a6 E6 t8 j9 yDetermine using the cold vapour atomic absorption technique. Select a
4 @: [3 [1 Q4 C: t, G( X. a5 n4 Hsample size appropriate to the specified level+ P& s. P8 \( V+ D
TESTS
' Z: c# N8 g. KPURITY TESTS
2 m; h4 M8 C$ R7 XImpurities soluble in 0.5 N1 s2 e8 y/ T0 j8 Q( A
hydrochloric acid
. A4 D# i4 h- B- Y; zAntimony, arsenic,
% c* ^7 u U S0 N Q$ P$ Kcadmium and lead
. [% x7 H. v+ S1 S(Vol.4)
2 @0 f6 B) @8 j& x$ N, wTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
. A* c; d- f3 |0 V$ n6 ohydrochloric acid, cover with a watch glass, and heat to boiling on a1 R9 M/ T2 b2 K; H
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
" \% M* R, C q1 Ecentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved* u0 O0 |8 c8 }
material settles. Decant the supernatant extract through a Whatman
" e0 E5 {: Q& ~ O. lNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
) S8 E2 x. N& ]0 {4 evolumetric flask and retaining as much as possible of the undissolved+ D3 e" ]. \. [7 R9 l+ F
material in the centrifuge bottle. Add 10 ml of hot water to the original
, D- S. X- V1 |/ xbeaker, washing off the watch glass with the water, and pour the3 X- ?3 ~, R+ Z2 C t
contents into the centrifuge bottle. Form a slurry, using a glass stirring( r* J9 [$ M7 r# B9 ]
rod, and centrifuge. Decant through the same filter paper, and collect
% ]7 E. w# ]7 @8 B+ @the washings in the volumetric flask containing the initial extract.
6 U# h+ v1 }/ D$ w" l: ZRepeat the entire washing process two more times. Finally, wash the: m! g6 o3 v- n1 x1 y) y2 S
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask! i5 q& S9 P, I) I5 c/ n
to room temperature, dilute to volume with water, and mix.6 p: V+ J+ H7 ?" A, D
Determine antimony, cadmium, and lead using an AAS/ICP-AES: ~4 ^/ d& I- l8 [9 P* |4 u3 t
technique appropriate to the specified level. Determine arsenic using the
! b, t7 y) ^3 h) aICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
; w {# O# u' z gMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
, E; B. z5 J( M y' i) E: a1 g. The selection of sample size and method of sample preparation
7 f# d# q0 l6 _may be based on the principles of the methods described in Volume 4.' |9 r( Y& ?, O
Aluminium oxide Reagents and sample solutions2 ? E8 p" Q m e0 y) E0 n
0.01 N Zinc Sulfate
$ s' ]1 |" J) ?4 k, [Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to$ @* z% ^, @5 J* A2 r- i
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
$ L$ C. N7 o+ Z. _7 j) Pof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
6 ~# f) G# W9 p3 [" Yconcentrated hydrochloric acid, heating gently to effect solution, then
2 S0 l; _! H/ u$ Ttransfer the solution into a 1000-ml volumetric flask, dilute to volume" u# k7 J: B$ j7 L6 K" A! }) A
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
% c1 c1 r- k4 w" E- g" ?7 k3 Tml Erlenmeyer flask containing 90 ml of water and 3 ml of' P' w1 K2 s9 |5 e
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
7 i3 P. [$ U* i8 T U; l25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,5 W# g3 d+ L. Z7 U
dropwise, ammonia solution (1 in 5) until the colour is just completely
* m3 D: a |9 x- K# i7 F* S1 gchanged from red to orange-yellow. Then, add:
" _3 Y4 r# J7 J/ ?* s3 R(a): 10 ml of ammonium acetate buffer solution (77 g of
3 `; t" D! z# y- E9 bammonium acetate plus 10 ml of glacial acetic acid, dilute to
9 \+ [9 h% c$ U) ?1000 ml with water) and( x+ I9 J# n: x9 y
(b): 10 ml of diammonium hydrogen phosphate solution (150 g' V0 h+ F+ J8 X7 G$ I# C" {* M
of diammonium hydrogen phosphate in 700 ml of water,) I8 d' _" T% n: o" {& x
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
/ Y2 u c2 ~# j( ]: w3 gthen dilute to 1000 ml with water).* V: f( E+ H1 P
Boil the solution for 5 min, cool it quickly to room temperature in a
, @5 { E+ x0 L% Z& w0 k" R8 _0 estream of running water, add 3 drops of xylenol orange TS, and mix.
) S9 C8 j, @, w4 j- BUsing the zinc sulfate solution as titrant, titrate the solution to the first
# `* {4 ]1 ^' t3 G! H; syellow-brown or pink end-point colour that persists for 5-10 sec. (Note:8 `- @4 s9 L- B2 X- c! d9 I* `: T
This titration should be performed quickly near the end-point by. d8 ]4 h0 ]/ X$ h, }
adding rapidly 0.2 ml increments of the titrant until the first colour
1 `# w" J3 V8 n1 V' t% d5 @, Pchange occurs; although the colour will fade in 5-10 sec, it is the true
) S5 t$ j% V# z s0 nend-point. Failure to observe the first colour change will result in an
" ?5 i$ h; s: E* A3 ~$ t- w$ x2 Qincorrect titration. The fading end-point does not occur at the second
6 o) u) }3 O7 K/ }" |( X) iend-point.)
$ x* ]& t3 Y' |7 ~% B* cAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
r( a8 b) t* x! h$ }' h. y, Ustream of running water. Titrate this solution, using the zinc sulfate
. h o) Z3 a1 o2 Z% Psolution as titrant, to the same fugitive yellow-brown or pink end-point
3 o- v3 i2 I, b# v6 T9 fas described above.
) s, ~+ M9 b) v. p) F( K0 GCalculate the titre T of zinc sulfate solution by the formula:
9 f+ D* `7 l5 @2 J: {1 C( j* w, ^T = 18.896 W / V9 d+ _- ~8 l# _4 a" @
where
% R4 {3 a: f- oT is the mass (mg) of Al2O3 per ml of zinc sulfate solution7 F9 c1 z- U5 M; N. B0 e- V
W is the mass (g) of aluminium wire9 [- {4 z- F: K/ z" r1 h* L
V is the ml of the zinc sulfate solution consumed in the* ]" J/ V0 N! M% N* z
second titration0 K' B# D! x0 c7 |9 m
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
6 d+ \0 z: W- j3 l. h% j, w4 Z$ QR is the ratio of the formula weight of aluminium oxide to
5 N y3 {' O5 Hthat of elemental aluminium., a/ B+ {) I& |: I$ f* o; d2 Z
Sample Solution A! }. ^! ]" f& N
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
/ r1 B0 k& D5 c9 p0 N9 k, mglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
! v' n) D0 w8 n6 B T+ _(Note: Do not use more sodium bisulfate than specified, as an excess
* w! H2 X8 n2 U3 h7 d! Hconcentration of salt will interfere with the EDTA titration later on in the% \& x, d0 C! S/ G/ d, q
procedure.) Begin heating the flask at low heat on a hot plate, and
8 p u( Q# o0 c: C0 h) @then gradually raise the temperature until full heat is reached.% p5 w. l" w1 Q1 B
(Caution: perform this procedure in a well ventilated area. ) When2 ^/ \6 @2 q. a
spattering has stopped and light fumes of SO3 appear, heat in the full
. y6 S9 }# ]+ L, Cflame of a Meeker burner, with the flask tilted so that the fusion of the; g! r3 U( \, S. J( }9 M( y, A
sample and sodium bisulfate is concentrated at one end of the flask.
* b% ~, T) e0 f) t0 a* oSwirl constantly until the melt is clear (except for silica content), but
; |% @& N5 Q- O" D& G1 Xguard against prolonged heating to avoid precipitation of titanium
) a3 H8 _( O8 K1 U% [1 J! ^dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
# k' }7 W7 S& j& Kthe mass has dissolved and a clear solution results. Cool, and dilute to
! v+ C O2 O& ^ ?120 ml with water. Introduce a magnetic stir bar into the flask.; k1 g. z' f- S! c1 s" { f* Z
Sample Solution B$ Q. p) \3 [4 a/ F
Prepare 200 ml of an approximately 6.25 M solution of sodium$ ~, E, e3 x/ Q3 a' d" M9 ?' F
hydroxide. Add 65 ml of this solution to Sample Solution A, while5 u/ w( ]/ ~$ ?, L# \/ a
stirring with the magnetic stirrer; pour the remaining 135 ml of the7 Z# m" [- ~; o( D ]! T/ P
alkali solution into a 500-ml volumetric flask./ _9 ?* o- J6 q+ y9 H. ]9 S
Slowly, with constant stirring, add the sample mixture to the alkali5 R# s5 X+ ]( h0 d, q
solution in the 500-ml volumetric flask; dilute to volume with water,
5 C+ t7 f) n0 |$ q7 L2 Hand mix. (Note: If the procedure is delayed at this point for more than
8 U1 J9 p* \+ S% l2 hours, store the contents of the volumetric flask in a polyethylene( x0 G' m5 K N) h- T) \
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),( T) Q) }+ X: h
then filter the supernatant liquid through a very fine filter paper. Label* `8 H% E0 c6 G1 s, S9 K8 E. s. [
the filtrate Sample Solution B.- o; }8 Z1 _& n8 s- I
Sample Solution C
. q7 {3 i% s- b9 @Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer5 ^4 E$ m( b8 `1 E, {, o
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid. `5 |- z7 A6 z; L" t( _" F
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
- J1 D1 w& q* {/ ~5 MM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
) N) a8 _; ^* y% @# dknown, calculate the optimum volume of EDTA solution to be added' [* x* G1 E; r
by the formula: (4 x % Al2O3) + 5.]5 \) X/ @6 D6 e! N# C
Add, dropwise, ammonia solution (1 in 5) until the colour is just
) H: N7 F$ D' Z+ e6 o4 f Q# xcompletely changed from red to orange-yellow. Then add10 ml each
, t7 S' D" u8 B$ c5 Cof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to* W. Q; s, n& c5 x [( \
room temperature in a stream of running water, add 3 drops of xylenol
7 W; M7 A* Y; B9 \0 @orange TS, and mix. If the solution is purple, yellow-brown, or pink,
8 B/ `6 I' v& S% F+ C: O5 |1 ]bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired# I. t( S ?4 \2 O
pH, a pink colour indicates that not enough of the EDTA solution has$ w( A8 ? k. p
been added, in which case, discard the solution and repeat this- g) p! {% l( K: t
procedure with another 100 ml of Sample Solution B, using 50 ml,0 w# x) j8 U+ J$ Q
rather than 25 ml, of 0.02 M disodium EDTA.
+ z- I# M6 l; E. _* z) YProcedure
7 A/ [9 B2 z: N" S# H$ E+ _Using the standardized zinc sulfate solution as titrant, titrate Sample
( U8 {, h8 Y! ?2 x, P$ H6 SSolution C to the first yellow-brown or pink end-point that persists for
( i+ I4 A; i1 I5 j+ x ]2 f5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
% Y6 G& l8 c# `; f# W$ c5 etitration should require more than 8 ml of titrant, but for more accurate
8 ^! _! Z9 N9 B2 nwork a titration of 10-15 ml is desirable.
0 i2 ?5 a. I6 c. ^0 ?, Q! C0 VAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5! u+ d) B G. M6 H( Z6 W* \5 I- L
min, and cool in a stream of running water. Titrate this solution, using
' A- F+ t1 q1 t; N0 U! lthe standardized zinc sulfate solution as titrant, to the same fugitive3 O4 R" C4 p! U& s6 X& I3 q
yellow-brown or pink end-point as described above.+ E' _" c, ]3 u3 d+ X
Calculation:# h! C5 _1 }8 \
Calculate the percentage of aluminium oxide (Al2O3) in the sample7 r+ ?- ~" M a* p/ `, j
taken by the formula:
& }" I+ ?; S# [( R+ O% Al2O3 = 100 × (0.005VT)/S
0 k0 b I! U5 a4 I& x$ Mwhere5 a6 Z1 l6 l# F, D/ o: R
V is the number of ml of 0.01 N zinc sulfate consumed in! }- O4 x4 q8 V% \
the second titration,
& g5 q+ E9 i7 M7 ?T is the titre of the zinc sulfate solution,
! J1 n7 r& p9 ~& p3 C, l* `S is the mass (g) of the sample taken, and
! n4 M0 v) b% [0 ~! ~! Q0.005 = 500 ml / (1000mg/g × 100 ml).
+ Z6 {0 ~" H+ L: {Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
* [6 |2 i. Z Z& Q( n8 J# Kglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
" ~0 s6 P3 ~3 Z, r7 o7 `' S) t" HHeat gently over a Meeker burner, while swirling the flask, until
* F! ?3 [1 i" z3 v. `decomposition and fusion are complete and the melt is clear, except
" C6 m4 b3 q1 F/ s! Qfor the silica content, and then cool. (Caution: Do not overheat the3 P0 Z! c8 w+ j% W
contents of the flask at the beginning, and heat cautiously during
2 c: `! k5 x O" o' d. ~% Pfusion to avoid spattering.): ~2 k) P3 l- f9 r6 f. S7 q
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat3 a# n1 D: ]4 n! A( Q
carefully and slowly until the melt is dissolved. Cool, and carefully add
! c; D" G- I8 S0 X) V* N. q150 ml of water by pouring very small portions down the sides of the
9 L: `& p; M4 p# Q1 U( `9 C- G2 qflask, with frequent swirling to avoid over-heating and spattering. Allow( w. f* O' |0 p) Z. q0 r
the contents of the flask to cool, and filter through fine ashless filter
T6 V/ ?0 N$ b/ _+ n1 h+ Q. hpaper, using a 60 degree gravity funnel. Rinse out all the silica from
+ B3 V6 k! \* Z K( \3 P+ F/ [the flask onto the filter paper with sulfuric acid solution (1 in 10)., U8 D0 M0 C( s
Transfer the filter paper and its contents into a platinum crucible, dry in
) Z0 ? u# a6 e6 V) X$ \an oven at 1200, and heat the partly covered crucible over a Bunsen
7 w" b( t5 z6 U8 a( O+ P' n* ?' ]burner. To prevent flaming of the filter paper, first heat the cover from0 c& o- ]4 U$ o! Y& A
above, and then the crucible from below.
, w/ X& |5 F9 gWhen the filter paper is consumed, transfer the crucible to a muffle
+ @, e- E8 Y* P& Sfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
& R5 v! C$ E0 g6 m% Iweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
1 ]! m6 Y& ^8 \, I$ Khydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first; j d$ h5 g5 z' A) t, v& j3 ^! `" s
on a low-heat hot plate (to remove the HF) and then over a Bunsen6 m1 [; V+ V; C+ t% I. Z* n8 y
burner (to remove the H2SO4). Take precautions to avoid spattering,
1 n/ S" i8 H/ w" I( l, ^5 b( k0 Uespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a! O& C# @% P& b
desiccator, and weigh again. Record the difference between the two% Z5 H. _5 g/ B" C( Y
weights as the content of SiO2 in the sample.9 ? V8 L+ N: f
METHOD OF ASSAY$ B4 T) \7 S2 `; w5 n' b
Accurately weigh about 150 mg of the sample, previously dried at 105o
+ L1 Q; \' a7 N# |) K9 X$ ^) qfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
. y% w% r# O) d# U Xand shake until a homogeneous, milky suspension is obtained. Add 30' S/ F. t8 k' `0 ^
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
) o# T" [4 P: ^' ~- H" k1 K: Iheat gently, then heat strongly until a clear solution is obtained. Cool,
9 s* E1 ?$ f* w% ]( Tthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric( \' q: P% } z& ]/ y6 \2 Z4 u
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
H7 m2 G. K# f# K+ C; N% brubber stopper fitted with a U-shaped glass tube while immersing the0 U! X# n! q4 c4 [7 ~+ b
other end of the U-tube into a saturated solution of sodium
5 x. X# p6 ~, Abicarbonate contained in a 500-ml wide-mouth bottle, and generate4 v! j* }. d# ]2 s
hydrogen. Allow to stand for a few minutes after the aluminium metal% ?# u4 p7 ]9 ^* q& Q# Y1 o
has dissolved completely to produce a transparent purple solution.: q9 z) p ]( F* U ]+ C F/ x
Cool to below 50o in running water, and remove the rubber stopper
1 X( w0 r. H/ Y7 z! {carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate. \" v# N4 M9 m( h" b
solution as an indicator, and immediately titrate with 0.2 N ferric7 [1 i, {, M; V- {# E; h
ammonium sulfate until a faint brown colour that persists for 300 g1 |! p$ [+ h8 |9 t, B4 [: Q
seconds is obtained. Perform a blank determination and make any4 G$ q, L+ l1 N. X
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is2 n0 r* q& v) A
equivalent to 7.990 mg of TiO2.
* X" @9 L) z+ [! Y+ T0 } |
|