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二氧化钛(钛白粉)
二氧化钛(钛白粉)/ X! X2 v& ]" S
$ [$ ?7 ?0 A" W2 ZJECFA关于二氧化钛(钛白粉)的结论
# }) h8 c; {% W3 ~/ ]0 s' T8 d/ _7 ?9 l0 x
摘要: 2006年JECFA关于二氧化钛的结论
2 r# F+ }8 ^! \6 J7 [3 _% }ADI值:不作限制。
. T5 @ ]# _* c) f! d# d' ?功能:着色剂' V# a2 c9 F [4 s4 C/ s7 C
% [3 S' y" v% ^8 f2 b A% d6 [
TITANIUM DIOXIDE" W4 Z/ {* ^5 D2 i$ T4 V% r
Prepared at the 67th JECFA (2006) and published in FAO JECFA! Q' j" q$ x1 S3 {" H
Monographs 3 (2006), superseding specifications prepared at the 63rd
7 D& `7 h) Q' FJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
; @: z4 ]- a2 ~Combined Compendium of Food Additive Specifications, FAO JECFA2 K+ _9 x& g5 b; A
Monographs 1 (2005). An ADI “not limited” was established at the 13th
! Z1 H( X2 F3 AJECFA (1969).. v' J) D' k2 u9 p1 u3 K7 ]
SYNONYMS
, g- l/ S3 t5 ETitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171% R4 v+ s, P: V0 Y- n: T
DEFINITION4 g% q% l) p) t
Titanium dioxide is produced by either the sulfate or the chloride, f8 U" Z, e8 a0 Y# c8 F/ z) [
process. Processing conditions determine the form (anatase or rutile. e/ n6 t Q# O) d$ D" O; U+ j
structure) of the final product." a; L. N: Z9 t; O8 y; R& Z
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)& F1 n4 u3 A1 H+ M; J
or ilmenite and titanium slag. After a series of purification steps, the
4 K& f1 P& i$ b: ~, O; Z& \isolated titanium dioxide is finally washed with water, calcined, and. V2 E; e6 h+ ~! c5 T/ l( [
micronized.0 P, g6 ^* e% m
In the chloride process, chlorine gas is reacted with a titaniumcontaining B' l7 ?+ J' Y. w$ k; G
mineral under reducing conditions to form anhydrous
" Q+ N5 y- j# |6 L/ I/ _$ Y: Gtitanium tetrachloride, which is subsequently purified and converted to- b+ I/ o3 S: _1 x. x. S; X) Z# o" F
titanium dioxide either by direct thermal oxidation or by reaction with* B' R% }1 J3 O2 `
steam in the vapour phase. Alternatively, concentrated hydrochloric
C( R+ G' W( M4 l+ k5 s1 r, Zacid can be reacted with the titanium-containing mineral to form a- l! f& O# h, z! }. o. L
solution of titanium tetrachloride, which is then further purified and
0 p; T ~0 e% b$ [- b1 v1 Cconverted to titanium dioxide by hydrolysis. The titanium dioxide is! ?9 ]7 r x6 A$ h e4 U d
filtered, washed, and calcined.# v; e* N- }$ {1 J' N
Commercial titanium dioxide may be coated with small amounts of
$ Q9 I, _' A) B. L) Palumina and/or silica to improve the technological properties of the
5 D7 `7 t& H/ b5 N/ k7 X, kproduct./ H$ {4 I- _. ~0 Q
C.A.S. number 13463-67-7
6 i9 u" j) e1 Y# t& BChemical formula TiO2- b1 D9 ]6 j# ^2 V v
Formula weight! v7 O! F& h. `1 b' @" i& u0 z
79.88) ]3 V( z, z [
Assay s: Q. H1 M2 g9 ]/ `' n
Not less than 99.0% on the dried basis (on an aluminium oxide and/ e+ l' E6 U) \6 @% |* }1 `
silicon dioxide-free basis)0 i; I) `. _8 [+ X- }7 z0 e
DESCRIPTION
/ V5 t) h) i L, x+ tWhite to slightly coloured powder% ~: s. a& x0 G/ n! Z- T
FUNCTIONAL USES
7 m$ h/ }& G$ O0 B5 e5 }4 x8 AColour; D7 k% o9 Z$ _. k6 x/ X
CHARACTERISTICS
9 w, b$ c) @1 G9 r8 B' a- h, rIDENTIFICATION
( A2 d8 q7 ?: N& U# K7 P n$ L7 o) dSolubility (Vol. 4)4 T& k) W1 |* R) b
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
4 g5 c1 l6 d3 c( b, _" N+ xsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
# S; B* j* t6 E& e; H" Bsulfuric acid. D. c6 D- a( Z* B# k6 Y5 ? a
Colour reaction k" R. ^- T# q6 L& x
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of' e- L }% i& U' F' z6 z% a' e% J7 B
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
/ H! P4 x% i& q3 [8 Pwater and filter. To 5 ml of this clear filtrate, add a few drops of, Y6 T* O7 B# w D5 I9 v8 B0 }
hydrogen peroxide; an orange-red colour appears immediately.
# l+ Z u0 D& P" n t% pPURITY$ a$ A, B N! j+ X
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h); t, d7 k# w* q h" \% N5 J
Loss on ignition (Vol. 4): O& ]' }# y' ?+ ~# `2 o8 V
Not more than 1.0% (800o) on the dried basis6 M$ H' G' E- v+ a0 C
Aluminium oxide and/or7 [: E& U" q, u4 m# W: u7 Q3 R
silicon dioxide$ x' S4 E) O. O# Z
Not more than 2%, either singly or combined# p; x" r: R( Y& i; i5 C
See descriptions under TESTS- I i# L. C; ^2 ]/ p* J( n5 i5 o
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing6 y' X" J4 {" F( a
alumina or silica.
4 G1 a' {' [9 R! V2 Z( D VSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and* U" x( e8 ]3 R7 O! k
place on a steam bath for 30 min with occasional stirring. Filter" X, w7 [% \: X
through a Gooch crucible fitted with a glass fibre filter paper. Wash
y- W+ }" [0 v- I% o, Mwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the: }: c! M9 A1 c _- K" K
combined filtrate and washings to dryness, and ignite at a dull red
: w/ g- p: z' c, r t2 `heat to constant weight.
3 m5 A. Y8 i4 A7 sWater-soluble matter' Y- Q) w1 `- k! ?* b6 l
(Vol. 4)$ W; p$ x* b( Q3 C& }. y
Not more than 0.5%
; T- I. C$ c. _: ]+ CProceed as directed under acid-soluble substances (above), using6 B% Q% C# l& R, U
water in place of 0.5 N hydrochloric acid.
! ]2 {) n2 J: z8 e! o5 g& gImpurities soluble in 0.5 N% X. `. \0 n5 k D! ]0 U$ u; C
hydrochloric acid- S, \7 W7 \0 L( ]4 E Y
Antimony Not more than 2 mg/kg
) Z5 k% L" K8 l- _See description under TESTS
( C; q) I6 o5 ]3 N1 V. TArsenic Not more than 1 mg/kg
( p; U$ H5 B ?4 Q( ~) w4 uSee description under TESTS T4 q: \( H8 z* T
Cadmium Not more than 1 mg/kg
) p5 b( P& F8 L4 u3 A3 LSee description under TESTS5 H2 F" b; }4 k
Lead6 z4 h. N8 o' G( _: Q
Not more than 10 mg/kg
0 c; V: B8 b; X ]& aSee description under TESTS
2 Q& K& C! x: Y; n$ M' ?. T+ ^Mercury (Vol. 4) Not more than 1 mg/kg4 i, m1 r# Q/ R9 g" G* v
Determine using the cold vapour atomic absorption technique. Select a- u* K+ N3 {* W! Z. u, g9 S7 n
sample size appropriate to the specified level
2 R$ C% V$ o, D2 g: O2 ETESTS
# ~6 m# \) ?' E% wPURITY TESTS8 D7 `# ~. @) R% v- a
Impurities soluble in 0.5 N
3 w ?0 y2 x5 O+ N$ E' khydrochloric acid: x. m) {3 i" g% h% t. ^2 d
Antimony, arsenic,
6 A7 d u" e0 F: |- K+ Y9 rcadmium and lead' R# z9 v, F& {. f1 C% e' e# A' o* A
(Vol.4)
$ y( \( P0 j8 FTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
/ b# e# U w& H, o4 j' ]3 `hydrochloric acid, cover with a watch glass, and heat to boiling on a% c& x2 V& o" m% b9 {; K+ ~- T; d
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml: N8 U: z X3 J% N' J
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
* u( g+ P' J0 R6 Smaterial settles. Decant the supernatant extract through a Whatman
. y% Y+ Y" z( o9 V4 T$ QNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
( j* S& o8 O( i& r1 Lvolumetric flask and retaining as much as possible of the undissolved
7 L0 @ A" h4 mmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
0 j2 U- l4 B, u% abeaker, washing off the watch glass with the water, and pour the ]. k# c# P% ^9 o4 h ~
contents into the centrifuge bottle. Form a slurry, using a glass stirring; k6 G5 r" S6 h$ [! L
rod, and centrifuge. Decant through the same filter paper, and collect
% P/ n& t4 @1 v: N W* d2 V8 Q1 vthe washings in the volumetric flask containing the initial extract.
8 _9 q H7 v* GRepeat the entire washing process two more times. Finally, wash the
- K \! ^! S; z K! }filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
) I- y# n; g) K3 h* q) O5 ~& Eto room temperature, dilute to volume with water, and mix.3 s3 b) K# i2 H9 U8 }: c
Determine antimony, cadmium, and lead using an AAS/ICP-AES
8 v7 ?2 ]7 O- F8 q% e0 B) h$ F" c: etechnique appropriate to the specified level. Determine arsenic using the
: A3 H9 p. h5 EICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
7 U! X* ], s8 _' G& S7 |5 ~Method II of the Arsenic Limit Test, taking 3 g of the sample rather than" w% A" U k" }0 W U
1 g. The selection of sample size and method of sample preparation7 s" k# v8 }) K$ }; \ a4 b
may be based on the principles of the methods described in Volume 4.
: {6 h8 v" n5 AAluminium oxide Reagents and sample solutions
5 `& N+ K9 L7 T+ i, e v7 l0.01 N Zinc Sulfate
, A# c5 j D. ?5 D" D9 x( m2 wDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
1 T1 _: L3 _" {- b6 D1 V vmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
# B9 w. `, p0 Aof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of; b- l+ M: b% m' q% ]8 q8 Z
concentrated hydrochloric acid, heating gently to effect solution, then3 u3 ]3 v( a8 f4 G" j% o
transfer the solution into a 1000-ml volumetric flask, dilute to volume( U3 B! D1 M0 o+ C& t4 f
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500' u, U9 J9 N! ?$ |; |3 g$ E2 M9 z
ml Erlenmeyer flask containing 90 ml of water and 3 ml of; P! q3 y: w+ y( `! _
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
' X- S# g$ }( |7 _, w7 C25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
1 ^( O( Z1 [, Gdropwise, ammonia solution (1 in 5) until the colour is just completely3 R) q, @& }# f: ?
changed from red to orange-yellow. Then, add:! u. g7 ^1 |0 |. d8 q
(a): 10 ml of ammonium acetate buffer solution (77 g of
/ `2 I G( g c+ Y' Bammonium acetate plus 10 ml of glacial acetic acid, dilute to: R5 g6 e* }& d
1000 ml with water) and j; D/ a! C# G- g* }# l( y. T
(b): 10 ml of diammonium hydrogen phosphate solution (150 g: [) l! Q \- S; Y9 E& S7 \) F0 G! N
of diammonium hydrogen phosphate in 700 ml of water,
5 X! h; I5 b$ F" d/ C$ c) k; @adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
8 P3 O! q! c2 ^then dilute to 1000 ml with water).
6 U, c6 V0 ?3 uBoil the solution for 5 min, cool it quickly to room temperature in a
8 L" n5 N/ h M; i4 o' ~stream of running water, add 3 drops of xylenol orange TS, and mix.
1 n) P* j* n. WUsing the zinc sulfate solution as titrant, titrate the solution to the first
6 u" ~: d6 E9 m8 yyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
9 a; h. D) Q1 s8 l7 i7 x8 ~This titration should be performed quickly near the end-point by Q$ a: ]$ M' V; J2 N
adding rapidly 0.2 ml increments of the titrant until the first colour
" m3 m q; a! S5 O( Pchange occurs; although the colour will fade in 5-10 sec, it is the true \7 o( X8 B3 o/ o& n% _/ I
end-point. Failure to observe the first colour change will result in an
6 J$ Y8 _+ R; l. t% ?% zincorrect titration. The fading end-point does not occur at the second
6 F1 [# \7 \% a Gend-point.)
4 V6 ?$ f4 p: g5 |" B8 [Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
0 s2 t2 g; U: a0 T# Hstream of running water. Titrate this solution, using the zinc sulfate0 q- I0 W7 c Q' N; H$ }
solution as titrant, to the same fugitive yellow-brown or pink end-point5 s/ \: C+ @% F' P" _2 @
as described above.
0 k. ?& B6 a4 X& R. ?Calculate the titre T of zinc sulfate solution by the formula: X; `0 |4 O$ W% s$ g7 T
T = 18.896 W / V
+ {2 s1 Q% O. w! G0 U) Vwhere
; k/ s, B D, v" JT is the mass (mg) of Al2O3 per ml of zinc sulfate solution; Z+ g9 |# e5 U9 b4 g1 ]
W is the mass (g) of aluminium wire( |( i Q& `5 r# y8 S% a A
V is the ml of the zinc sulfate solution consumed in the* A* X0 i z, t+ J& p/ _
second titration
$ {, [. k5 n* e0 i$ E% j& \18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
& N9 p* b* k& c% t! t1 oR is the ratio of the formula weight of aluminium oxide to
0 m6 |& x' I- \; ~: o( `" tthat of elemental aluminium.
% P, v% U+ @; }( k9 LSample Solution A
* T- @. k- h- g! h! j9 lAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
{% _* h$ |5 L6 }glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
* e+ w( q2 ^7 x) A; Z, d(Note: Do not use more sodium bisulfate than specified, as an excess# n" O. m. a6 c3 J% I9 d
concentration of salt will interfere with the EDTA titration later on in the) o3 s, k2 A0 K! l5 y5 ?) F
procedure.) Begin heating the flask at low heat on a hot plate, and
0 o& q/ Y. S0 g+ [1 i+ U+ hthen gradually raise the temperature until full heat is reached.
- Z( ^- {" M& H# @. R; g% z7 H {(Caution: perform this procedure in a well ventilated area. ) When' i. M' y }, ?$ @! ?6 q# Z
spattering has stopped and light fumes of SO3 appear, heat in the full2 G0 @+ S* N4 P E/ _
flame of a Meeker burner, with the flask tilted so that the fusion of the
* ?) z7 D% ?1 c) p1 b) e; [sample and sodium bisulfate is concentrated at one end of the flask.# H; p: H% T: q
Swirl constantly until the melt is clear (except for silica content), but
- ^! {& |5 _$ }1 ^' p0 t) [guard against prolonged heating to avoid precipitation of titanium& q/ G* c; Y; @: H3 ]
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until. P, C5 D6 l+ b! S0 g( z" l
the mass has dissolved and a clear solution results. Cool, and dilute to
& t3 y |/ ]* }8 M9 @& u2 A* t120 ml with water. Introduce a magnetic stir bar into the flask./ E( G! e r ~4 E
Sample Solution B, _) E# u6 T% z- P
Prepare 200 ml of an approximately 6.25 M solution of sodium
* h' Z/ f7 C/ lhydroxide. Add 65 ml of this solution to Sample Solution A, while6 A% g) ^5 ~; g1 D( y
stirring with the magnetic stirrer; pour the remaining 135 ml of the" C$ P; ]7 w _ }" N( _ E
alkali solution into a 500-ml volumetric flask./ [0 \& |5 n$ r2 X: p! {
Slowly, with constant stirring, add the sample mixture to the alkali
. U4 V' U% | t. Jsolution in the 500-ml volumetric flask; dilute to volume with water,/ t( B, ~/ n m# X' U
and mix. (Note: If the procedure is delayed at this point for more than
' A. M/ l, g4 b" Y" g% Y2 hours, store the contents of the volumetric flask in a polyethylene
8 ~7 g" m2 |! ?5 X$ Tbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),0 _6 w0 s6 R" G* ^
then filter the supernatant liquid through a very fine filter paper. Label
; H) O8 a9 e2 d+ A* s" _8 q" ?1 othe filtrate Sample Solution B.* i/ z; F6 G; M: N8 d; J. f$ e. F) G
Sample Solution C9 {* i6 r/ J1 h# F7 ]( f4 z
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer# `% @0 Z v0 f7 U1 [& I( J
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
: T7 B$ U7 @7 v% K4 K' Ysolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
! O0 r5 Q% c3 r4 `' EM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
' A( V+ H$ o) J2 eknown, calculate the optimum volume of EDTA solution to be added
2 k w8 v2 w, P& ?3 [) i' C; Lby the formula: (4 x % Al2O3) + 5.]
, k5 S! ?" ]+ a. hAdd, dropwise, ammonia solution (1 in 5) until the colour is just
* U( v5 q2 w& d X, n3 @completely changed from red to orange-yellow. Then add10 ml each
4 O4 w8 z" C/ C# F0 T9 r% O: dof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to5 y& D' |1 F; _* Y: G! L
room temperature in a stream of running water, add 3 drops of xylenol' O: S7 L0 W ^1 l
orange TS, and mix. If the solution is purple, yellow-brown, or pink,6 v& _1 v) P5 r; x: M
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired& ^1 O) R* e. W5 d
pH, a pink colour indicates that not enough of the EDTA solution has% ?7 o0 D u& G" P" K7 b
been added, in which case, discard the solution and repeat this, l; m) E, z! G- q9 B& h- ^
procedure with another 100 ml of Sample Solution B, using 50 ml,
3 r! `7 Y7 t: G6 Rrather than 25 ml, of 0.02 M disodium EDTA.
4 b d; k. M' S4 i/ }3 G# wProcedure
n8 O! ?7 \+ GUsing the standardized zinc sulfate solution as titrant, titrate Sample
" x' X, D9 D; V( cSolution C to the first yellow-brown or pink end-point that persists for1 h! K, G2 c* b
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
# `) H2 z& [' I: y: V: A* Stitration should require more than 8 ml of titrant, but for more accurate w, w9 e/ q* L0 H& ]9 \# W0 V& j
work a titration of 10-15 ml is desirable.
. ^3 C7 D# W5 f8 }+ wAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
" o* i0 z: x/ Q" Rmin, and cool in a stream of running water. Titrate this solution, using
1 \9 S# H! ]. ?the standardized zinc sulfate solution as titrant, to the same fugitive* }2 M* G5 ~2 d* ?: a) Y
yellow-brown or pink end-point as described above.
/ F6 X4 y: G3 b) U: F' m& SCalculation:
k. W' C* S( f' Z iCalculate the percentage of aluminium oxide (Al2O3) in the sample1 n% U m' U1 L3 ~2 P- {5 X
taken by the formula: |& H9 J' B" w* n! s& u
% Al2O3 = 100 × (0.005VT)/S- U* u$ y7 u# m. C" W. x
where
) F0 Z9 [# V% DV is the number of ml of 0.01 N zinc sulfate consumed in# M; G' g/ G, w6 z
the second titration," j9 N5 J0 i9 _% O( {" e9 z
T is the titre of the zinc sulfate solution,; e* T! Y. ]1 ?( r6 [9 A! H
S is the mass (g) of the sample taken, and; E. |7 s$ }9 z. a/ t
0.005 = 500 ml / (1000mg/g × 100 ml).3 A8 `7 r9 v0 H# ^: |& W
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
( S' l- e* R5 Oglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).' k# U5 i3 i( ]5 }7 }$ b
Heat gently over a Meeker burner, while swirling the flask, until) ^9 B+ u8 @$ T; F4 y% ?! A; a
decomposition and fusion are complete and the melt is clear, except
& {1 c' [! m P8 M7 @( r7 p3 ~for the silica content, and then cool. (Caution: Do not overheat the
. v5 N9 V- R D1 k1 Fcontents of the flask at the beginning, and heat cautiously during
8 _3 S: C8 Y0 \' [2 }fusion to avoid spattering.)
8 V* ^4 D: k8 k! O8 X; \; }, MTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
" ^9 w C9 a N* t! g& G' Ncarefully and slowly until the melt is dissolved. Cool, and carefully add
. r& m; G/ ~0 i" T, t) J150 ml of water by pouring very small portions down the sides of the
6 b, {% _, d ~+ k& |flask, with frequent swirling to avoid over-heating and spattering. Allow
4 n O# D2 T4 xthe contents of the flask to cool, and filter through fine ashless filter# X- w9 N8 c. k. s
paper, using a 60 degree gravity funnel. Rinse out all the silica from1 a' k) {, |; K* @7 g4 b
the flask onto the filter paper with sulfuric acid solution (1 in 10).; D c5 g: N# E
Transfer the filter paper and its contents into a platinum crucible, dry in
* N1 ]3 }# o: K2 u3 @8 r! {- \an oven at 1200, and heat the partly covered crucible over a Bunsen
9 X- @& [0 u& h& O2 q/ rburner. To prevent flaming of the filter paper, first heat the cover from5 V+ S7 ^" a# W8 n4 u$ s3 R
above, and then the crucible from below.
% m( h# p) [. r% D6 {When the filter paper is consumed, transfer the crucible to a muffle* q( {' r! @" h
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and+ J( p0 N& w/ Y4 |# }
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
" y6 K, B* b A* C* U& _; t C% Chydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
$ Z: J! B2 r8 y2 D: Don a low-heat hot plate (to remove the HF) and then over a Bunsen
! f8 C7 U3 O2 w- e0 uburner (to remove the H2SO4). Take precautions to avoid spattering,
) }& v' F, H! V' s$ k9 n# O6 ?especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
6 o+ F0 M3 f) Jdesiccator, and weigh again. Record the difference between the two4 @# Z3 n" D9 t) G. x2 ]% o
weights as the content of SiO2 in the sample.% }! x! ]5 a0 @* c* b
METHOD OF ASSAY
, V% N6 j5 e8 ], e2 { ~) }, TAccurately weigh about 150 mg of the sample, previously dried at 105o
9 }! _ K/ x1 V8 y9 V* F4 t. }- tfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
0 M4 _6 C k Z# w3 { nand shake until a homogeneous, milky suspension is obtained. Add 30
$ L E( n: w* l) q6 w6 Yml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially& A: \, R, j' r# [
heat gently, then heat strongly until a clear solution is obtained. Cool,
% H$ `7 J d! [8 C. ~then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
8 k+ |: v' K4 h& ~& q* A$ K0 dacid, and stir. Add 3 g of aluminium metal, and immediately insert a% p! O. j) j; J8 E) r% C4 A$ H
rubber stopper fitted with a U-shaped glass tube while immersing the
7 W, o7 @- C5 y J9 l7 m+ Sother end of the U-tube into a saturated solution of sodium
( O, Y; D3 N9 k1 _0 Fbicarbonate contained in a 500-ml wide-mouth bottle, and generate
* P3 \6 `/ C) {) [hydrogen. Allow to stand for a few minutes after the aluminium metal
! F$ V8 |" `5 \# E) N) lhas dissolved completely to produce a transparent purple solution.
4 S, c K9 u2 `- I( w" yCool to below 50o in running water, and remove the rubber stopper
4 |( O+ e/ Y7 G1 n Scarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate! W3 |) X' x' C8 k4 t* e' K
solution as an indicator, and immediately titrate with 0.2 N ferric
0 x* T P' Q- y3 {1 ~" @+ v$ r% nammonium sulfate until a faint brown colour that persists for 309 W7 c( l- S! T- A- K/ {
seconds is obtained. Perform a blank determination and make any t: _0 `9 D# V9 h& q. f
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is2 s. g k- V# q4 A
equivalent to 7.990 mg of TiO2.
. {' N' Q! \$ Z; U |
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