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二氧化钛(钛白粉)
二氧化钛(钛白粉)
B; b* a, v7 ~8 b' w" B! H3 d5 _
JECFA关于二氧化钛(钛白粉)的结论
8 |9 `! B7 T# u/ c7 A" D+ _1 D7 a7 a5 @6 s$ m; i5 x, \
摘要: 2006年JECFA关于二氧化钛的结论
5 y' `+ H" L3 k3 Y0 P% NADI值:不作限制。
4 _( B% z7 y0 b! w5 {' b% Z功能:着色剂
! |* p* q; T' I9 r) ?8 ~* ~$ ?) X* Q* M: s1 b
TITANIUM DIOXIDE& K( s8 m) y3 |$ ? r# e
Prepared at the 67th JECFA (2006) and published in FAO JECFA
" ]: Z3 W5 X* [# _/ c. Q% y9 u) XMonographs 3 (2006), superseding specifications prepared at the 63rd
( F4 y; r' N8 H7 `. EJECFA (2004) and published in FNP 52 Add 12 (2004) and in the) A6 e( K+ G9 ^1 c u
Combined Compendium of Food Additive Specifications, FAO JECFA
! P: g q! g& r& ^; x' p- L# o$ gMonographs 1 (2005). An ADI “not limited” was established at the 13th: O' F0 t' _9 c- l. M
JECFA (1969).
* h/ ^6 f0 d& a4 T8 x) g7 ESYNONYMS
7 ^# b! s B0 U- l1 G+ i: A, Z7 UTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
. `( ~2 T1 q. n r1 `DEFINITION
) Z$ u5 [, k! \6 \Titanium dioxide is produced by either the sulfate or the chloride
$ s7 i) e# I4 q' p0 ~* c* Lprocess. Processing conditions determine the form (anatase or rutile# y! f; G( X$ B- P4 Y ?
structure) of the final product.
3 C+ d8 P4 n9 N0 Z6 QIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)- `2 \& E" y0 R1 U9 @: O
or ilmenite and titanium slag. After a series of purification steps, the. h* x! v+ H6 {# J5 h+ x I
isolated titanium dioxide is finally washed with water, calcined, and; H- s3 F' f0 k
micronized.
9 m4 |0 V& @. g1 W9 T, FIn the chloride process, chlorine gas is reacted with a titaniumcontaining
# d; k% s1 j$ D' _9 g! Cmineral under reducing conditions to form anhydrous" }! \8 W/ k4 `& Y2 V' ~
titanium tetrachloride, which is subsequently purified and converted to5 k( ]9 ~, j* K8 o; O* ]$ P3 P4 u
titanium dioxide either by direct thermal oxidation or by reaction with
" s5 I' y# o9 o$ r) |steam in the vapour phase. Alternatively, concentrated hydrochloric9 M1 D1 v, Q' |$ L' M* b( y
acid can be reacted with the titanium-containing mineral to form a" _/ K6 \% [6 g' S/ g
solution of titanium tetrachloride, which is then further purified and* v' U3 _0 J8 b6 H+ M9 x" |& x
converted to titanium dioxide by hydrolysis. The titanium dioxide is
% ~4 E2 O0 ]- Z9 efiltered, washed, and calcined.7 s7 B( X& g0 q- O+ v
Commercial titanium dioxide may be coated with small amounts of
7 Z' j1 c+ }# g5 falumina and/or silica to improve the technological properties of the
1 P1 h1 X/ c3 {2 Y4 \3 @product.
% l: z y: @0 DC.A.S. number 13463-67-70 d8 Z6 ?& p4 [9 u. P
Chemical formula TiO20 Y3 \# l! d6 Y! P0 f2 u, s
Formula weight, P- A2 p7 |. ^' R) X. d
79.88
9 ]0 {' k7 g0 ]Assay% `& D. A4 L9 P
Not less than 99.0% on the dried basis (on an aluminium oxide and3 W, O2 c% r" e2 ]
silicon dioxide-free basis)
: b8 S& j; ~1 J. |; x6 {3 ^DESCRIPTION, u/ h% h- _/ f' \' l9 P& ^
White to slightly coloured powder
4 I8 f" v# m/ y9 jFUNCTIONAL USES* `! B& }! E+ n" }# E" \# Y X! y
Colour
5 m( r" l- M2 z' c* Z3 i. a' }CHARACTERISTICS
; B, S( ~' c# Y5 E, S }- JIDENTIFICATION
) r% z7 m- Q# K) ^Solubility (Vol. 4)
/ N& {% Q* o. S6 X5 i( X4 p/ rInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
$ f) ?/ _: Y6 x' w( a Zsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
; C, L5 u' d' O( t6 nsulfuric acid.7 |2 W( x1 f( q' X
Colour reaction Q: E }& ~# i( q6 {
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
6 G( }! Q4 |! Q& k- psulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
$ b- ?& m& b! y5 T9 K lwater and filter. To 5 ml of this clear filtrate, add a few drops of. e% i S- l. [1 F0 y
hydrogen peroxide; an orange-red colour appears immediately.
, r% h5 U4 r! C8 G5 K: kPURITY1 m! M; h& o# x0 c5 g8 r: u ?
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)! s+ L- g: _7 f* j
Loss on ignition (Vol. 4)8 m4 ?$ V) K4 u- P' s
Not more than 1.0% (800o) on the dried basis4 f3 a. J" {: M1 Y/ \ `
Aluminium oxide and/or
: @3 P2 z: }" y Y3 msilicon dioxide
4 l/ I/ n: d4 Q2 ONot more than 2%, either singly or combined
4 V: p# f$ d: K6 cSee descriptions under TESTS
0 v" h5 V, Z3 z+ ?- e$ ~Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing+ U4 ]6 W. X& Q$ D8 ^% R* l
alumina or silica.+ L0 N5 s* y( ]
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
! O6 L" b+ m `- l- splace on a steam bath for 30 min with occasional stirring. Filter
7 i( L8 u5 I d4 r, a# N8 s/ g- gthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
/ j0 x* L B$ Y2 Dwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
( Z+ |/ e5 I! x1 o+ Z( v) }combined filtrate and washings to dryness, and ignite at a dull red: u J8 N* @2 G
heat to constant weight.
, C- v9 C7 d5 A# X( i, gWater-soluble matter
4 {" T4 T- t9 x z- t5 h(Vol. 4)( I# z) c% y) ^1 F2 S
Not more than 0.5%) p7 {1 X- k0 @+ }0 E
Proceed as directed under acid-soluble substances (above), using% S! k. q3 w: Z, C; p" c0 p
water in place of 0.5 N hydrochloric acid.: R5 V: |5 e2 |/ P7 v P- u
Impurities soluble in 0.5 N
1 a$ \' Y' o) z6 z M6 B g/ Z/ zhydrochloric acid
& F2 p+ ` ]/ F% A/ H. r4 C8 SAntimony Not more than 2 mg/kg
+ _8 f9 t. N5 u0 u% c) Z' C, c7 B9 f9 JSee description under TESTS* Y* f+ }2 ]5 X6 ]& ` ?3 \! ~
Arsenic Not more than 1 mg/kg" X+ h8 N/ j: I2 L [' F
See description under TESTS$ T2 _- j" W9 q& e- v3 [! _0 T/ F5 @
Cadmium Not more than 1 mg/kg8 F. m+ |1 o8 N5 i" H, }+ M K
See description under TESTS
* l: Z [4 g! |Lead T$ {3 D1 v) ~: L
Not more than 10 mg/kg4 ]9 {& A. Y+ h( b# L% j
See description under TESTS7 o5 }" e" w+ E& C+ z0 }
Mercury (Vol. 4) Not more than 1 mg/kg8 z$ l4 M$ s" `/ q* ]! N
Determine using the cold vapour atomic absorption technique. Select a0 i5 b' @ ]5 \/ ?
sample size appropriate to the specified level
9 ?7 g+ y, s6 `' qTESTS
' {+ _3 }6 c+ w; L" Q4 q. ?PURITY TESTS% k1 f# z; t* t% S6 `, j
Impurities soluble in 0.5 N
" i' O% i* i( z5 L6 w& l5 ?hydrochloric acid3 \' f* y2 [7 ]$ E. P. O
Antimony, arsenic,+ a/ `9 i/ _2 ^: i" ]
cadmium and lead
' q3 n. F! W8 Z1 V8 ~2 u/ L/ P: \(Vol.4)
) n- U6 Y- j: Z2 u k8 Z6 o* JTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N3 G/ I6 `. I! E
hydrochloric acid, cover with a watch glass, and heat to boiling on a
8 e# i. }4 Y$ Y0 e1 t9 Dhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
9 U' |4 Y! s- t9 L/ o' ~1 C+ bcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
# G( V# G3 s3 h4 `, Fmaterial settles. Decant the supernatant extract through a Whatman
) l( \6 j3 h4 u5 gNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
- E0 a% b2 @& R* f' f# Cvolumetric flask and retaining as much as possible of the undissolved
$ U) b+ b3 m; A5 x2 C, |6 Tmaterial in the centrifuge bottle. Add 10 ml of hot water to the original* R3 Q! S; T9 W. p
beaker, washing off the watch glass with the water, and pour the2 s9 e5 u' B. Y) h& i9 ]5 {9 w z
contents into the centrifuge bottle. Form a slurry, using a glass stirring, ?" x" \/ W% H) E$ t
rod, and centrifuge. Decant through the same filter paper, and collect
! Q& c8 Z9 Q9 M% mthe washings in the volumetric flask containing the initial extract.
. ]2 K( E- a! P( z2 v) i8 DRepeat the entire washing process two more times. Finally, wash the
- c4 _' \" d8 R# }' V- P* E+ \filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
% w& P& m4 f, z8 g* T% Uto room temperature, dilute to volume with water, and mix.; U' k8 ?* O. L
Determine antimony, cadmium, and lead using an AAS/ICP-AES
" Z5 s! m$ b7 M6 p% j, _* W5 Ptechnique appropriate to the specified level. Determine arsenic using the
8 x/ _+ s# `0 g4 Z* ^ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using0 n8 L* h* H+ ]
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than- c, n" v9 e- g& t
1 g. The selection of sample size and method of sample preparation" q" B- X% j0 _ y; |
may be based on the principles of the methods described in Volume 4.% p9 H! N* W" Y5 x' w, }1 H
Aluminium oxide Reagents and sample solutions
2 m$ Q4 `! B" X& Y0.01 N Zinc Sulfate
8 A4 f5 b" l( x+ qDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
( l9 z8 W" c% f6 P3 ~) a& D4 g' emake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
$ z+ z# @# _: X6 k6 Y9 nof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
' V% t7 r; B3 s4 R. e. [concentrated hydrochloric acid, heating gently to effect solution, then
) o3 ~2 K1 R- @transfer the solution into a 1000-ml volumetric flask, dilute to volume0 u3 {& W1 g% [
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
; R# [" e+ }! z' tml Erlenmeyer flask containing 90 ml of water and 3 ml of
0 c6 G+ C7 Z& xconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
8 u4 t1 d! e H' ~, t( U* j25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
- G( V5 \8 O1 T# z: ydropwise, ammonia solution (1 in 5) until the colour is just completely
0 V2 b) j' U' C, f) L: \) Tchanged from red to orange-yellow. Then, add:
" [5 A F1 ?& W4 c- [(a): 10 ml of ammonium acetate buffer solution (77 g of
; w& q7 D2 q- Q/ hammonium acetate plus 10 ml of glacial acetic acid, dilute to- x& {- F" N' x) a
1000 ml with water) and6 q2 S7 Q1 G) I( M* o. b5 B
(b): 10 ml of diammonium hydrogen phosphate solution (150 g" Z+ G, q g q V% d
of diammonium hydrogen phosphate in 700 ml of water,
* h1 q6 a; P& g/ \adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
5 r: V# U- u5 o& |" a0 ithen dilute to 1000 ml with water).% y* H! b) E, v# L3 [! L5 f
Boil the solution for 5 min, cool it quickly to room temperature in a
. `: b3 I$ g+ Z, h* U4 {1 sstream of running water, add 3 drops of xylenol orange TS, and mix.
' E- B& _9 R# t* b" |% w3 |% ZUsing the zinc sulfate solution as titrant, titrate the solution to the first( U+ n# y/ B3 r* c9 O+ J" r7 c7 n
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:8 @( H" y( [+ k# { w$ J; k
This titration should be performed quickly near the end-point by1 o9 o; p4 R7 ?, m
adding rapidly 0.2 ml increments of the titrant until the first colour
' Y' m( u1 ^. @! ~( z$ zchange occurs; although the colour will fade in 5-10 sec, it is the true
& P. h5 |% f# O7 lend-point. Failure to observe the first colour change will result in an- j) x$ a0 O R# K# J
incorrect titration. The fading end-point does not occur at the second: D0 B" V. T% V4 z! Y6 L
end-point.)
' ~+ ]) c0 K1 h$ M/ }5 D: c/ TAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
: `0 P* ?' ~* V$ X, Istream of running water. Titrate this solution, using the zinc sulfate; N7 o2 ^' h6 l: O3 ]
solution as titrant, to the same fugitive yellow-brown or pink end-point; s( f6 h1 O9 Z9 S; w
as described above.3 a: u% C% a. Y. ?( i
Calculate the titre T of zinc sulfate solution by the formula:
1 w( a' J2 Y& XT = 18.896 W / V/ ?' H+ G& R! O! |
where
0 E/ t. b! S4 ^# g# zT is the mass (mg) of Al2O3 per ml of zinc sulfate solution2 v0 k- _7 z8 d5 b" G$ {: x
W is the mass (g) of aluminium wire
7 b! ?3 i& n4 [' \, W7 `5 WV is the ml of the zinc sulfate solution consumed in the
" I: j( @( ~( c. jsecond titration
! Y/ ~$ f7 o5 M( R* |6 B$ Q, @& H18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and5 j7 o$ Z1 h( q' W0 n# ?
R is the ratio of the formula weight of aluminium oxide to, P6 E& W. Y. F' R
that of elemental aluminium.8 \! ~% b' k1 r- y) k
Sample Solution A
" z W& V% ^4 y; k: w- X7 `+ TAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
5 ^/ ~ M2 I. T* }* v4 O( r$ Vglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
3 x+ }5 f! ^. k" {$ K( m(Note: Do not use more sodium bisulfate than specified, as an excess
7 R6 M& X0 `/ w% Zconcentration of salt will interfere with the EDTA titration later on in the
( U% \9 @2 S+ j3 eprocedure.) Begin heating the flask at low heat on a hot plate, and( w! ~- f0 L& V, M" ~+ ?
then gradually raise the temperature until full heat is reached.
0 m# Y) w4 N3 z. A(Caution: perform this procedure in a well ventilated area. ) When
+ n: H+ D5 x. u* o7 a. Ispattering has stopped and light fumes of SO3 appear, heat in the full
/ L, S/ m3 V3 k5 J: q8 q: }flame of a Meeker burner, with the flask tilted so that the fusion of the0 j. d! d! V/ {
sample and sodium bisulfate is concentrated at one end of the flask.
* Q9 t5 ?- J8 Q L' H6 s5 ]Swirl constantly until the melt is clear (except for silica content), but
. @5 A0 T" r) vguard against prolonged heating to avoid precipitation of titanium
n* {9 A' C$ M& Q5 e3 Y! Gdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until1 e" F$ F) C7 w
the mass has dissolved and a clear solution results. Cool, and dilute to
5 L8 v% ^3 i5 M) k' D8 C& T120 ml with water. Introduce a magnetic stir bar into the flask.
1 }, D; v9 t1 _* w- nSample Solution B- ?# j6 e" e0 i+ Z
Prepare 200 ml of an approximately 6.25 M solution of sodium
% @8 A" e7 D w8 E, dhydroxide. Add 65 ml of this solution to Sample Solution A, while5 X1 B( ], Z# h8 g9 }, L; t( |
stirring with the magnetic stirrer; pour the remaining 135 ml of the8 P4 S* d: l- M7 o$ s/ i7 X
alkali solution into a 500-ml volumetric flask.
# ?) K* U# y. [6 B8 SSlowly, with constant stirring, add the sample mixture to the alkali
( T! p7 k: C5 I* J9 Hsolution in the 500-ml volumetric flask; dilute to volume with water,' B& W9 T* d7 u9 f7 z5 v0 n% c. {
and mix. (Note: If the procedure is delayed at this point for more than
- h! u: c1 [) Y" H/ f2 hours, store the contents of the volumetric flask in a polyethylene8 \ w( f1 G9 T% @
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
2 ^8 r; M9 e+ p8 E' a( e! tthen filter the supernatant liquid through a very fine filter paper. Label$ ^" m, ]+ @0 b# P( x
the filtrate Sample Solution B.& D# _7 C) h G1 ~8 ]+ R8 b
Sample Solution C9 Z6 J2 e9 d; r! n
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer& A( p. h5 D9 }& L8 G: d( i( F; e
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid; M% p/ v1 z' C8 m/ H- f
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
9 E8 t2 {" f& W) w. N$ dM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
, T9 v9 x' d' _' y/ ~" R* `3 Pknown, calculate the optimum volume of EDTA solution to be added
8 ? y- v9 g zby the formula: (4 x % Al2O3) + 5.]
' [+ Z5 Y: L# rAdd, dropwise, ammonia solution (1 in 5) until the colour is just
( [$ m& [" h) t3 acompletely changed from red to orange-yellow. Then add10 ml each
: h$ q& k; z- w8 a4 y$ ~5 R/ jof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to. Q3 W+ z8 _- e' e6 b5 l5 v( k
room temperature in a stream of running water, add 3 drops of xylenol9 O1 Y# A' e6 s, E5 s W9 {
orange TS, and mix. If the solution is purple, yellow-brown, or pink,( [! C! e) J) a B! ?: z
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired8 R3 E6 `+ F1 V. k4 a$ y1 D* a" {
pH, a pink colour indicates that not enough of the EDTA solution has+ C3 A4 d A7 ]2 n4 e6 O. O
been added, in which case, discard the solution and repeat this3 l; B; Y* {, ]! d
procedure with another 100 ml of Sample Solution B, using 50 ml,
* @! O2 W4 }" j* ?4 }8 _rather than 25 ml, of 0.02 M disodium EDTA.9 N4 `( d& ~# q/ @% Y4 B
Procedure, m' T1 ]" L3 M4 l
Using the standardized zinc sulfate solution as titrant, titrate Sample+ J P' o( N: Y+ h4 d# q
Solution C to the first yellow-brown or pink end-point that persists for
' q. ?6 F+ Q& B8 e& n. X$ o5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
' E, s5 W( o( E3 Btitration should require more than 8 ml of titrant, but for more accurate+ S. |- a e% i8 w! d/ v
work a titration of 10-15 ml is desirable.
0 I0 e& a6 p. GAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5( q: A/ P0 I6 K% |1 n
min, and cool in a stream of running water. Titrate this solution, using
7 M! o7 [' L4 g+ E: l. o7 U0 jthe standardized zinc sulfate solution as titrant, to the same fugitive6 J" U4 e( N) Z+ r+ E0 {
yellow-brown or pink end-point as described above.
7 l U4 B5 _( u3 ? l- {Calculation:; E% f4 Z" @$ m! @% d. w- Q6 c
Calculate the percentage of aluminium oxide (Al2O3) in the sample
3 r! X* ]- }9 }: o' Z! Btaken by the formula:, } u% k# x& s* S5 B A, c2 j
% Al2O3 = 100 × (0.005VT)/S
) z+ ]8 \8 x; wwhere/ ?, d& R. s; ~: Z9 g
V is the number of ml of 0.01 N zinc sulfate consumed in) A! w" C+ D* u& M# j4 [
the second titration,
3 Q) N5 K. T5 R I7 L6 {7 l2 x, o6 X% HT is the titre of the zinc sulfate solution,
% e8 w) S4 B, n, k/ u7 WS is the mass (g) of the sample taken, and
7 i3 P0 d3 u1 l0.005 = 500 ml / (1000mg/g × 100 ml).
' C7 [: C8 ~8 L9 RSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica- l. K" z. D4 f5 l5 [ e
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).1 _7 S/ F8 s7 B& x( B$ d, _
Heat gently over a Meeker burner, while swirling the flask, until( t# D n( b- n7 C. }
decomposition and fusion are complete and the melt is clear, except5 J- q: J3 v {) ?
for the silica content, and then cool. (Caution: Do not overheat the
, y% i7 M# F1 z# b v% |contents of the flask at the beginning, and heat cautiously during6 p, e& M6 G+ D4 M& a
fusion to avoid spattering.)
; }, @" R4 D/ q! G# ?6 ZTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
~. E( P* \% P n# F0 ?carefully and slowly until the melt is dissolved. Cool, and carefully add& W# j8 d$ k1 M$ H2 a' l$ _) `
150 ml of water by pouring very small portions down the sides of the) |1 L! g* U' C& V9 d) y! s
flask, with frequent swirling to avoid over-heating and spattering. Allow
% G2 }' @+ R3 l& Hthe contents of the flask to cool, and filter through fine ashless filter7 A+ Y! o; N, |
paper, using a 60 degree gravity funnel. Rinse out all the silica from
* S# Z3 a" ~; ?, q4 d. uthe flask onto the filter paper with sulfuric acid solution (1 in 10).
4 {9 V4 s, g4 V2 t0 v4 T" LTransfer the filter paper and its contents into a platinum crucible, dry in
4 S) [/ C8 v# e. c3 tan oven at 1200, and heat the partly covered crucible over a Bunsen
9 W6 b+ |5 }7 C( h0 y# eburner. To prevent flaming of the filter paper, first heat the cover from
: S: Z" h6 R8 E) O9 l/ b8 b, Xabove, and then the crucible from below.
3 Y) e/ F! e! L9 s4 j+ pWhen the filter paper is consumed, transfer the crucible to a muffle
3 e8 v; D! ~+ n# jfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and- u+ u( Z2 J: y+ j; F8 }* Z7 A
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated7 p$ \5 W* c o
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first8 y2 t- b9 J) ~# a" U. g$ C" W
on a low-heat hot plate (to remove the HF) and then over a Bunsen# A& [8 b5 a; [* p: W6 ~1 S, j
burner (to remove the H2SO4). Take precautions to avoid spattering,
1 \5 U( b5 o7 d+ o9 _3 u7 I' eespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
) x5 e5 T1 b) S' O& y0 B$ \desiccator, and weigh again. Record the difference between the two2 ?+ c- b" C9 Z( B/ C/ S% J" i
weights as the content of SiO2 in the sample.2 s+ Q, D6 y7 U5 E- q6 H
METHOD OF ASSAY3 o+ D2 r3 a, b
Accurately weigh about 150 mg of the sample, previously dried at 105o
) f: z# F5 z7 h& Nfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
# M5 A! E/ Z1 A0 W( z! j8 E4 a' Y4 J% Xand shake until a homogeneous, milky suspension is obtained. Add 30' V0 I% w3 i! q; h8 Y
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially' G4 m$ r- s; g0 K2 b% S
heat gently, then heat strongly until a clear solution is obtained. Cool,
( u1 y: \! I; q# bthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric: L( @* m. u! b( {
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
& G5 f1 r K# V2 D( x! rrubber stopper fitted with a U-shaped glass tube while immersing the# `1 i1 V. e* _5 i5 l
other end of the U-tube into a saturated solution of sodium9 V- `6 D0 b) \/ Z
bicarbonate contained in a 500-ml wide-mouth bottle, and generate: r2 ^9 ?/ t6 Q9 g: X+ ^! c7 |* i
hydrogen. Allow to stand for a few minutes after the aluminium metal l" e/ b9 L3 e4 u
has dissolved completely to produce a transparent purple solution.
8 @/ V" w, F+ [Cool to below 50o in running water, and remove the rubber stopper: l$ i& u6 X- x8 k& t
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
% G1 X1 X5 K# G& ]solution as an indicator, and immediately titrate with 0.2 N ferric
+ B7 ~9 J3 H/ R. H7 S4 Oammonium sulfate until a faint brown colour that persists for 30
6 j1 w- T' N2 v" A) v+ F; d5 bseconds is obtained. Perform a blank determination and make any
% A6 \; t% i) \5 f3 Hnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
# J; E7 i L2 bequivalent to 7.990 mg of TiO2.% `' c" o' F7 n2 X
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