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二氧化钛(钛白粉)
二氧化钛(钛白粉)
# Y2 v, D6 W7 ?' g% H7 K% |
; p. i3 C4 P4 p$ nJECFA关于二氧化钛(钛白粉)的结论
7 ^7 |! ]6 Y6 L- w7 \7 B1 ]2 g+ X& m/ U( v" l
摘要: 2006年JECFA关于二氧化钛的结论& N S+ t/ g# G% Z' b
ADI值:不作限制。, Y! }7 |3 w( ?0 E1 s( O1 H+ x! l9 N
功能:着色剂! D2 R7 t% c# \: ^& A! \7 x
4 G" r( ^+ K9 s. H
TITANIUM DIOXIDE
2 H: @) S5 n* i+ B/ g, A cPrepared at the 67th JECFA (2006) and published in FAO JECFA
. ?) l3 D2 T* G0 W! rMonographs 3 (2006), superseding specifications prepared at the 63rd- a" J+ T" {6 D0 v. I
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the3 H* _( I$ `" m
Combined Compendium of Food Additive Specifications, FAO JECFA! g7 R, C. Y/ B
Monographs 1 (2005). An ADI “not limited” was established at the 13th& ]. X y( a! E, W
JECFA (1969).! f3 _9 z" o p% D, \
SYNONYMS6 o7 `) r: H$ I8 `' c; O
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
3 O3 k7 J2 Y& x2 n- J3 w4 [5 SDEFINITION
$ _ Y: o! X3 j. ]Titanium dioxide is produced by either the sulfate or the chloride
9 X) @. r. r8 W1 D# k! E3 r2 hprocess. Processing conditions determine the form (anatase or rutile1 w0 q; S! l5 u- C4 r+ k# S
structure) of the final product.
4 D5 W5 V: ?' [3 ?& l: HIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)! g) f* @9 Z5 h4 F# U D
or ilmenite and titanium slag. After a series of purification steps, the
& Q$ ]1 @# d/ y" K% E m' @; ~7 lisolated titanium dioxide is finally washed with water, calcined, and
4 W a9 h- {, ^" C' l* O2 w0 _micronized.9 m7 {3 J: J9 R- k* ^( S) t8 v
In the chloride process, chlorine gas is reacted with a titaniumcontaining
4 Q1 b$ a) `$ F$ ymineral under reducing conditions to form anhydrous
9 N F' o! g# Q' n& k/ q4 ltitanium tetrachloride, which is subsequently purified and converted to+ {; S% z0 M( U( L
titanium dioxide either by direct thermal oxidation or by reaction with( c3 @* A$ U5 y
steam in the vapour phase. Alternatively, concentrated hydrochloric: E8 _9 o8 o6 d: h3 k( d5 t4 b) k
acid can be reacted with the titanium-containing mineral to form a7 s9 n5 [/ N3 f- _
solution of titanium tetrachloride, which is then further purified and# b/ W) s0 u- I
converted to titanium dioxide by hydrolysis. The titanium dioxide is/ [5 w& l1 x1 K n9 M
filtered, washed, and calcined.+ B7 A9 I! j1 n% b( z
Commercial titanium dioxide may be coated with small amounts of, r) \1 T a) ~1 P. Q
alumina and/or silica to improve the technological properties of the
! S! ~8 {+ e4 `: l) n1 G. ]7 m, pproduct.
5 q& y8 F+ ~: T3 RC.A.S. number 13463-67-7
$ a8 Y4 Z3 p) B9 JChemical formula TiO2
- Y9 x n: h. h% {Formula weight& z8 d7 W S. ~3 d* C: \3 d
79.887 B/ j% y4 ?$ V5 N% D/ r. ^& v
Assay
$ w4 Y' r8 f" K( A8 F" {Not less than 99.0% on the dried basis (on an aluminium oxide and
! B% A! ?4 P, {silicon dioxide-free basis)$ ~6 o9 c8 N, z' m0 N& k% O
DESCRIPTION
) J5 O3 F- g F9 x3 a' F. w- YWhite to slightly coloured powder
3 h! y8 `* N* [8 a; R9 h( j. jFUNCTIONAL USES
; I) Z' i% W0 B7 bColour
8 j1 E! }% h/ m, J: t" SCHARACTERISTICS& |! y" ? l8 r" Y: A
IDENTIFICATION
4 u; V9 y) ^6 H5 ~8 VSolubility (Vol. 4)
& r' H* T2 I+ W2 @4 l# W* U: UInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
" K% s5 }! S* K! x& R2 msolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
* [; x: O5 e. I3 l; o" N8 E8 A: Usulfuric acid.. n2 O3 G) X, n9 k5 x5 L
Colour reaction
6 @6 ?; H3 k) a+ lAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
+ i% a9 c5 x) y6 }: F/ J9 F7 Lsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with% o0 E8 |) R2 ], j; T# x
water and filter. To 5 ml of this clear filtrate, add a few drops of, Y+ u+ j% p8 Z& \4 i6 }/ h) h
hydrogen peroxide; an orange-red colour appears immediately.0 w% t/ f& i# r$ W2 T9 r
PURITY
$ w2 d+ G% L/ H" b7 M* j: C. D7 W' o3 XLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)2 M6 y/ J4 k* Y3 J
Loss on ignition (Vol. 4)
9 @# K0 y- C- Z# b( qNot more than 1.0% (800o) on the dried basis0 f+ v" Q# @3 N; v% c
Aluminium oxide and/or
, l$ y1 F @5 ]( B) ~0 V5 bsilicon dioxide3 U* H9 C Z% X6 C0 X0 Q
Not more than 2%, either singly or combined' n; V0 @) Y- E& B
See descriptions under TESTS, a& `* o4 V% u7 ?7 }* y
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing! Q4 w, K5 k- K4 I" }
alumina or silica.
8 h0 y5 |* X: N% Y- |% {$ _( PSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and" ]9 J9 o+ Z# v x/ n& Q
place on a steam bath for 30 min with occasional stirring. Filter
2 u* g! g- x4 f4 m$ Sthrough a Gooch crucible fitted with a glass fibre filter paper. Wash7 n% ]5 ]9 G' l( ^- z" L3 s: l" N
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the( v' }. m4 f: M; p) |
combined filtrate and washings to dryness, and ignite at a dull red$ d: M9 |! A! f N; G
heat to constant weight.7 o& k/ q! K; ~9 X( l- U
Water-soluble matter2 X9 v0 C) o, D( B7 q- q9 |
(Vol. 4)
) W' e: L7 I! X& O3 HNot more than 0.5%
4 `) T z+ l& J. MProceed as directed under acid-soluble substances (above), using
0 {: ^ {# {# p4 f' V7 B* cwater in place of 0.5 N hydrochloric acid.
, f( F% d& |) O1 TImpurities soluble in 0.5 N1 Z8 i+ `& ~( t6 \! W8 p5 U. u
hydrochloric acid! D5 ]& A+ p/ W& d# S7 f6 e4 q
Antimony Not more than 2 mg/kg3 W! @ r) m$ g3 X
See description under TESTS5 J. Q {5 N# m, |4 R+ y
Arsenic Not more than 1 mg/kg
) R3 w" i( C$ f, J6 N" nSee description under TESTS
* d9 t& q* p" a+ E/ d- _Cadmium Not more than 1 mg/kg
" S! C4 i5 t( `0 j% lSee description under TESTS& j% A5 B2 v6 i0 e U, h/ j
Lead7 F9 \- ]6 M m8 E
Not more than 10 mg/kg
8 [# |3 x0 i& ]: Y, ~- [See description under TESTS
, P7 L. n0 V5 l9 ~/ u. DMercury (Vol. 4) Not more than 1 mg/kg
' p0 B; n5 F6 \6 O; T5 @Determine using the cold vapour atomic absorption technique. Select a$ B2 |' ~4 v; I
sample size appropriate to the specified level: X2 ~, Q7 C N- ?( _! i# `% x
TESTS& L8 c& t. e; _; ?1 @7 J% U3 J5 p
PURITY TESTS5 S6 w+ R! V7 D7 o2 |. q [
Impurities soluble in 0.5 N6 j! W0 ^4 M0 m6 f
hydrochloric acid
1 {$ X- G0 X, G' cAntimony, arsenic," d& g6 {! m a; _4 v
cadmium and lead
/ C) g. l9 n3 x9 m3 t( L9 E/ N( p(Vol.4)
- v5 r& g) T5 E3 H& T" F1 T; GTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
+ l3 p; i1 d& j) d( L1 a# Q# n0 m& O* phydrochloric acid, cover with a watch glass, and heat to boiling on a
* ` p; x; P; H3 F4 Q! m6 |' |$ Phot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml3 F' Y0 @6 i9 r: X, R$ v
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved* c [2 H1 G% B( J3 G8 a0 z& m
material settles. Decant the supernatant extract through a Whatman
7 J2 }: o+ q- I6 yNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml$ [$ h3 L, a6 H( I- k" b6 J: I
volumetric flask and retaining as much as possible of the undissolved
6 k# J; \6 q6 V" K8 v( j) q S) d8 T: x1 ?material in the centrifuge bottle. Add 10 ml of hot water to the original
/ o) ^+ O; V2 ?% G% L& @beaker, washing off the watch glass with the water, and pour the* j& O: X- X; t
contents into the centrifuge bottle. Form a slurry, using a glass stirring
9 L' a" T/ f" f! @- g' Brod, and centrifuge. Decant through the same filter paper, and collect
% k& e1 O) |0 r u4 Kthe washings in the volumetric flask containing the initial extract.% O& Q, Z' i2 `+ S7 p* [
Repeat the entire washing process two more times. Finally, wash the; i' @: g- ^2 W
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
6 ]6 L3 Z4 g; |to room temperature, dilute to volume with water, and mix.
) @2 j" a) Z; Q. y; E4 xDetermine antimony, cadmium, and lead using an AAS/ICP-AES6 J: ^/ \5 {8 t- s& t# b1 M
technique appropriate to the specified level. Determine arsenic using the
* s8 j) F; f QICP-AES/AAS-hydride technique. Alternatively, determine arsenic using3 _- D% R# Y F& F
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than- Z+ `5 j/ |/ \# C8 M% z) d
1 g. The selection of sample size and method of sample preparation
! O) U% o8 n% J1 X3 C: Emay be based on the principles of the methods described in Volume 4.
6 k: W# }1 I/ t" t1 \Aluminium oxide Reagents and sample solutions. x0 N, } h* F7 c
0.01 N Zinc Sulfate: J" m% S ?" O1 Y4 u
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
7 O! Y" e' o1 F* imake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
7 J5 L" C1 w# n) }, c Qof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
$ M8 {9 o. v# ~0 i2 T" ]concentrated hydrochloric acid, heating gently to effect solution, then
5 R" X/ M8 Q/ ~$ i* utransfer the solution into a 1000-ml volumetric flask, dilute to volume0 C( `% `/ G& e! b+ _) d
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5004 S) q; l* r3 z# { `+ p$ z
ml Erlenmeyer flask containing 90 ml of water and 3 ml of& T, h! |4 t. Y% I% {3 N
concentrated hydrochloric acid, add 1 drop of methyl orange TS and4 H7 j H, s3 o. a0 E$ x' J6 S1 J
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,! E8 G- n' _; b% L! p! O
dropwise, ammonia solution (1 in 5) until the colour is just completely9 K9 m. | E( R9 J) U/ f
changed from red to orange-yellow. Then, add:2 J) I+ n- G% L e/ F" N; Y
(a): 10 ml of ammonium acetate buffer solution (77 g of- ?5 r$ X' D1 H. k3 V
ammonium acetate plus 10 ml of glacial acetic acid, dilute to5 v, j' z9 I) L6 ^* a
1000 ml with water) and
3 t/ H7 D: b G/ d! w- v$ g(b): 10 ml of diammonium hydrogen phosphate solution (150 g
4 Q( O8 G9 }7 E1 t% A( `+ i4 Pof diammonium hydrogen phosphate in 700 ml of water,
" I k! ?. h" D/ ?, P% d& w# S4 J, `8 [; T2 Eadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
% U$ G" U3 K, h% pthen dilute to 1000 ml with water).
+ h! J1 T% D/ m/ ]Boil the solution for 5 min, cool it quickly to room temperature in a
, Y8 U5 z2 C7 N2 Y; x% Zstream of running water, add 3 drops of xylenol orange TS, and mix.8 b9 y/ l& ~; O7 k5 d
Using the zinc sulfate solution as titrant, titrate the solution to the first! P0 H9 ?2 c! a$ N% L6 J* ]
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
. i& R) j+ E4 N9 u+ Y% s- g) T& oThis titration should be performed quickly near the end-point by& R- d( |' N6 A% G/ Y
adding rapidly 0.2 ml increments of the titrant until the first colour# g- ^8 H! ^5 K0 Q- B: {' a9 v
change occurs; although the colour will fade in 5-10 sec, it is the true
- l( W" a5 a8 p v% xend-point. Failure to observe the first colour change will result in an
( }% D; F: Q9 _2 [* Oincorrect titration. The fading end-point does not occur at the second
6 D5 P1 L6 G) c) j- W; F& pend-point.)
- |$ O' |/ g) h9 G( @Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
. N& k; m' f# P( j+ W# Z4 k# u4 h5 Estream of running water. Titrate this solution, using the zinc sulfate' d. D" y/ P! K$ ^; ?4 N
solution as titrant, to the same fugitive yellow-brown or pink end-point
% l1 `7 w7 c5 H% u- U) S( Sas described above.
, U+ Q0 i4 j$ ?& O9 h. k$ r& I6 aCalculate the titre T of zinc sulfate solution by the formula:
3 X+ l1 c0 [, }# [T = 18.896 W / V
4 U4 G9 s0 W1 @where V2 C9 j5 x2 k; Q7 v9 v, R
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution8 `6 Q7 F/ G# H& n1 z
W is the mass (g) of aluminium wire- X+ @+ l$ ~. b
V is the ml of the zinc sulfate solution consumed in the
0 H* q% p$ S Y) t$ asecond titration
4 ? q/ A, v; e0 z18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
' I- a5 z4 L) N4 eR is the ratio of the formula weight of aluminium oxide to# y) B' N7 Y: J8 j* o
that of elemental aluminium.) N' l4 u5 g: G9 Z& w! v+ F
Sample Solution A5 [) Q8 ^3 c4 ~' z
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
( W6 u/ ?( V5 e6 t. {" Aglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
/ Y5 {1 N6 I+ o3 v/ j(Note: Do not use more sodium bisulfate than specified, as an excess# ~5 d1 h6 i$ \; e. u
concentration of salt will interfere with the EDTA titration later on in the) T8 ^0 Q# n2 K# o
procedure.) Begin heating the flask at low heat on a hot plate, and
+ \7 \+ \& z7 A3 f8 {: t9 n& Othen gradually raise the temperature until full heat is reached.% j3 m( s6 Y, Y& V/ V$ t
(Caution: perform this procedure in a well ventilated area. ) When! |. U3 h1 L6 E1 R: u) X1 z' }
spattering has stopped and light fumes of SO3 appear, heat in the full
7 ?2 t1 V5 T6 Gflame of a Meeker burner, with the flask tilted so that the fusion of the- k7 ?3 C9 ?. x/ f
sample and sodium bisulfate is concentrated at one end of the flask.
1 u/ B: B& {: v4 b1 }Swirl constantly until the melt is clear (except for silica content), but
' O, V: b; v) W! sguard against prolonged heating to avoid precipitation of titanium
& X8 x0 O- a1 x0 e6 }; t4 pdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until/ j8 ~( a) i% Y5 G a
the mass has dissolved and a clear solution results. Cool, and dilute to
0 c, g3 P$ J) @9 S) a5 k120 ml with water. Introduce a magnetic stir bar into the flask.
+ n; ^; l9 C; rSample Solution B
/ h0 n3 X& L) P, EPrepare 200 ml of an approximately 6.25 M solution of sodium2 r4 D$ _0 n! E: e* q. Q+ [
hydroxide. Add 65 ml of this solution to Sample Solution A, while6 [9 B3 Q: ]$ g8 x# X
stirring with the magnetic stirrer; pour the remaining 135 ml of the$ _* h) M7 ^& P- H' t/ _' S( Z
alkali solution into a 500-ml volumetric flask." A* s O3 r, O1 ^& s/ i( o" o
Slowly, with constant stirring, add the sample mixture to the alkali
" N8 a9 w+ d R/ B, K# B5 e( isolution in the 500-ml volumetric flask; dilute to volume with water,
8 ?7 u8 y) L, zand mix. (Note: If the procedure is delayed at this point for more than
8 b. ~ _* A- |2 hours, store the contents of the volumetric flask in a polyethylene
5 J7 A& i( _; X% {+ b+ Ubottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
) s9 s% n% [2 I, s# Lthen filter the supernatant liquid through a very fine filter paper. Label
2 _' W; Z% D' q! b5 ?% Q& othe filtrate Sample Solution B." k2 v9 g7 |/ P; u: n* Z
Sample Solution C
4 t, O( y" C( uTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
2 A$ z+ K9 n7 Q% A$ v9 a2 aflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid# }4 a( G' y$ o
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
1 u" {" o! T) S$ |M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is& o0 S4 J# Z, b( A1 G
known, calculate the optimum volume of EDTA solution to be added
5 P* d4 k- f- P- Cby the formula: (4 x % Al2O3) + 5.]. X% `: I$ B, T- Y5 [
Add, dropwise, ammonia solution (1 in 5) until the colour is just
! f4 ?. @# I# i: F) R) m8 [completely changed from red to orange-yellow. Then add10 ml each
& H7 H9 m* [% D, Y8 n/ ]: Q/ Uof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to1 I1 }3 {5 p, s% m0 y. R
room temperature in a stream of running water, add 3 drops of xylenol T" t* X, i; v- O" _( K. P; r+ Q
orange TS, and mix. If the solution is purple, yellow-brown, or pink,- t6 k a3 m, w3 H
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired2 m9 ?9 V" s. C% |' \+ j
pH, a pink colour indicates that not enough of the EDTA solution has, d2 S+ s3 }) ~3 _$ y0 b$ j4 R
been added, in which case, discard the solution and repeat this
: ~8 O; ~6 {, u# o* ?! ~0 Q% Vprocedure with another 100 ml of Sample Solution B, using 50 ml,; t$ | v" v/ `6 a. C0 b- v
rather than 25 ml, of 0.02 M disodium EDTA.! [0 w- m. S; ^; A$ A
Procedure
, i: E3 j! M o! Y0 `- mUsing the standardized zinc sulfate solution as titrant, titrate Sample
2 J2 Y7 h1 l0 E- J L+ H! Q" n& MSolution C to the first yellow-brown or pink end-point that persists for7 @' K* G; F3 y F
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
y }6 S9 h: G; Dtitration should require more than 8 ml of titrant, but for more accurate: n! ^6 i2 F3 q; ^ n @/ L/ k
work a titration of 10-15 ml is desirable.
2 G" K" D- J! }% Y- @Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5) }) m- R9 z: ]
min, and cool in a stream of running water. Titrate this solution, using- J0 K# e! k, {. |, {' h- E
the standardized zinc sulfate solution as titrant, to the same fugitive e# t. \) E0 h
yellow-brown or pink end-point as described above.. C( ~7 F6 l; [! X: g
Calculation:
4 f6 u3 F& F; X7 h+ R2 FCalculate the percentage of aluminium oxide (Al2O3) in the sample) ^% i& W3 [6 s" u. q5 O3 H+ M
taken by the formula:* u/ J7 G# R8 o$ e9 }
% Al2O3 = 100 × (0.005VT)/S
$ u4 _# G# f9 L) V v* h+ d% fwhere
" X- {( z: a4 Q/ z- cV is the number of ml of 0.01 N zinc sulfate consumed in: q$ z0 J: M1 k6 v6 L+ S, Q2 \: M, U
the second titration,: p6 x9 s% Z' a6 X! ?1 ^6 P$ r
T is the titre of the zinc sulfate solution,
- r& Y0 M* W) d* a" B+ e# xS is the mass (g) of the sample taken, and% A$ q. z- H' C4 P
0.005 = 500 ml / (1000mg/g × 100 ml).
- h7 t- m d" }/ t8 aSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
* W* h4 H( M" I6 p, D& m7 qglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).8 t6 X: ~9 \9 a* r
Heat gently over a Meeker burner, while swirling the flask, until
! [1 D& c1 ?+ P9 n9 J; Y' Q# hdecomposition and fusion are complete and the melt is clear, except/ C( k$ q) ]' A7 @; f4 S% T
for the silica content, and then cool. (Caution: Do not overheat the2 K. g8 _$ C& o% w
contents of the flask at the beginning, and heat cautiously during" \- ?2 W+ | e$ `( ~ r
fusion to avoid spattering.)
* t, @$ g/ @ T- s# S" ?To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
% J) M, v/ x5 Q5 F# e8 ^" K. Rcarefully and slowly until the melt is dissolved. Cool, and carefully add6 F# v" p/ f3 B8 L
150 ml of water by pouring very small portions down the sides of the
O- F) s5 T7 x; s& F M- g* pflask, with frequent swirling to avoid over-heating and spattering. Allow
$ P o, J0 G; k8 \the contents of the flask to cool, and filter through fine ashless filter
) }! S, X6 p! a1 u1 U; Jpaper, using a 60 degree gravity funnel. Rinse out all the silica from3 }5 m% H) P% M3 R/ f7 D5 V
the flask onto the filter paper with sulfuric acid solution (1 in 10)., ]" B% ^* Z$ O/ j0 w' e
Transfer the filter paper and its contents into a platinum crucible, dry in! k, }6 o- `& O5 `' s
an oven at 1200, and heat the partly covered crucible over a Bunsen
8 _, H$ F: t3 K: cburner. To prevent flaming of the filter paper, first heat the cover from
/ I* u% }. D5 ^9 d+ w, R7 d) Xabove, and then the crucible from below.
8 I$ T$ `8 }3 C! |% u+ a0 Z2 RWhen the filter paper is consumed, transfer the crucible to a muffle0 H0 h) O9 S7 d- |1 |8 i
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
& T; V" o! H; \& |# J4 I6 kweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated/ m' Q8 k) m" K! F# C6 }4 m. {
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
' Z2 \: ~% c$ W' t$ u- h0 w9 Con a low-heat hot plate (to remove the HF) and then over a Bunsen1 `/ h% R+ H3 a7 _4 F
burner (to remove the H2SO4). Take precautions to avoid spattering,
2 e+ e6 w- _$ G- tespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a8 p# C; T4 F9 u4 A
desiccator, and weigh again. Record the difference between the two5 h1 U! d1 v2 V) b/ T) W* D
weights as the content of SiO2 in the sample.: d0 @+ O0 d1 r3 G9 S7 s
METHOD OF ASSAY
& }" w8 E& K2 L5 }% \/ eAccurately weigh about 150 mg of the sample, previously dried at 105o
8 c. U9 {5 a' U- ]( {( L Lfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
1 b# w' M$ U# ^( l6 \' U7 Xand shake until a homogeneous, milky suspension is obtained. Add 30% \3 ~2 a/ `. b( b M9 C# h
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially% n8 k9 g* F$ P; a! m2 d( U
heat gently, then heat strongly until a clear solution is obtained. Cool,! y9 d7 T0 U+ ^) `+ u- h: e) t
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric- H; ~8 P* ^. G4 P6 k0 @; ?
acid, and stir. Add 3 g of aluminium metal, and immediately insert a$ { }9 c8 s& \# S4 i
rubber stopper fitted with a U-shaped glass tube while immersing the
9 q& d2 z+ f# qother end of the U-tube into a saturated solution of sodium! Y3 j4 O" ?, [8 G, A3 ^. I
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
( D/ Z% }+ q& v3 X) r, Uhydrogen. Allow to stand for a few minutes after the aluminium metal
& }) E7 @; \! Whas dissolved completely to produce a transparent purple solution.
7 B0 {/ u6 v4 B' h0 DCool to below 50o in running water, and remove the rubber stopper
! i. N1 X/ _, Y/ F1 tcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
) u: i2 L! B2 k0 asolution as an indicator, and immediately titrate with 0.2 N ferric; P% V0 ~+ R- l- i
ammonium sulfate until a faint brown colour that persists for 30* e/ m$ W' [! B, t& |8 A7 y
seconds is obtained. Perform a blank determination and make any
5 j+ a, n9 w0 Z k" K0 C0 V0 J; wnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is- [' M6 q( ?. b' C) F
equivalent to 7.990 mg of TiO2.
' \& Y2 D0 l! [% Y |
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