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二氧化钛(钛白粉)
二氧化钛(钛白粉). ]- V# W+ W+ U3 v
& @8 `; V3 x( z8 g3 n
JECFA关于二氧化钛(钛白粉)的结论
- c3 z9 y5 h x0 w4 _& j, I, o& d- {; y9 \% `5 H2 | v4 A
摘要: 2006年JECFA关于二氧化钛的结论
2 @2 ]/ K2 O- h; L# j4 yADI值:不作限制。/ k- X! t( G, D5 n; b
功能:着色剂9 j! Q3 b! n: Z
# L7 S$ {* @( g' PTITANIUM DIOXIDE! `8 i& X( C, j; c
Prepared at the 67th JECFA (2006) and published in FAO JECFA6 P5 c3 @* A1 X, `* P- ?
Monographs 3 (2006), superseding specifications prepared at the 63rd k) E8 |: I9 c+ R9 \9 }
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the* w3 K" m& [& A, }
Combined Compendium of Food Additive Specifications, FAO JECFA
/ [* H0 A7 ~ Z- A- B) N# B1 PMonographs 1 (2005). An ADI “not limited” was established at the 13th1 x, N. b: M0 V* v
JECFA (1969).
2 ?1 `( b! E7 J% R% j/ M/ l" M( ~% qSYNONYMS
* m+ e) f7 {' R; e+ Y& sTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
" S8 R# s* g1 vDEFINITION
: \" A5 Q: @: g' l9 }Titanium dioxide is produced by either the sulfate or the chloride2 ~- U# N, X8 H; P* z2 D
process. Processing conditions determine the form (anatase or rutile$ i8 g; U# Y: ?2 i q$ Y
structure) of the final product." D9 b1 U+ R$ t
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
4 I) v4 q8 D; d* X* ?) hor ilmenite and titanium slag. After a series of purification steps, the
3 z0 }& w: i( v' r( f( M2 @8 Y9 Eisolated titanium dioxide is finally washed with water, calcined, and
; }1 J5 A2 S9 x. ?; A, r8 [! emicronized.
& j& z) E" R& A" o$ Q$ ^In the chloride process, chlorine gas is reacted with a titaniumcontaining
& r! z, L/ q! A" Pmineral under reducing conditions to form anhydrous
, w& H3 D$ G6 k& w2 k2 wtitanium tetrachloride, which is subsequently purified and converted to
. U3 p6 L: X1 A5 `! |titanium dioxide either by direct thermal oxidation or by reaction with
, A( S' v) M: G* D2 h* S( Ysteam in the vapour phase. Alternatively, concentrated hydrochloric$ J j, K! L* P9 O. J
acid can be reacted with the titanium-containing mineral to form a
; d! b9 m( a6 R; esolution of titanium tetrachloride, which is then further purified and9 {$ S5 N9 {# ^- M
converted to titanium dioxide by hydrolysis. The titanium dioxide is8 J" |0 g# g6 D3 w
filtered, washed, and calcined.
/ n$ s* F J0 H# G% w9 q" \Commercial titanium dioxide may be coated with small amounts of3 L+ c! d5 D/ F: A0 i3 [
alumina and/or silica to improve the technological properties of the8 v* u. D" ?5 I1 r6 k1 J
product.
) U w1 t, ^6 u) y( X7 FC.A.S. number 13463-67-79 `4 F1 c+ I+ r7 `7 H# B
Chemical formula TiO2+ u# G. T- N$ p# Y4 c
Formula weight3 ]9 ~+ b+ D3 S" V* j
79.88
) K* i0 T& v( R# s/ m) xAssay3 j9 K7 `3 ]& a6 |
Not less than 99.0% on the dried basis (on an aluminium oxide and3 n7 \" A: D2 y3 v7 T$ `( ^
silicon dioxide-free basis)
2 @" C( ^# z" S( n( ]DESCRIPTION6 U* z6 y" x& z a- ]& X
White to slightly coloured powder
; u* I% t: I. n6 z3 X5 rFUNCTIONAL USES
; a+ Z$ X, F5 y0 t8 YColour
& o* F1 x) O* W; RCHARACTERISTICS
0 p' n( h- M5 f$ m) t+ W6 OIDENTIFICATION
- G5 F6 b& h( c6 bSolubility (Vol. 4)! h& z! t4 p# k6 E
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
) E0 r( x# W* r2 Isolvents. Dissolves slowly in hydrofluoric acid and hot concentrated0 R3 g3 D$ x# d" `6 b1 }& z0 O
sulfuric acid.4 W E! ^+ L; N+ B+ _, j( K
Colour reaction
; ~ r* O# s9 D4 G6 w9 q |& wAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
: G( i1 V2 s' r* h a3 Xsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
. p2 g+ t9 i/ a; j/ Iwater and filter. To 5 ml of this clear filtrate, add a few drops of
$ p) h& y2 v" O2 S }( o. Y2 Ihydrogen peroxide; an orange-red colour appears immediately.) M8 E: z; ]9 n0 k2 C" C
PURITY, s8 Z# n0 N3 `% T; w$ n7 j" x
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h). o; E- |3 h9 k5 \5 f- r# e( m
Loss on ignition (Vol. 4)
5 o; l# v0 n" P# r& M6 U+ }Not more than 1.0% (800o) on the dried basis8 E0 c- ~" K6 R; ~- @; K
Aluminium oxide and/or
i+ {1 o' I2 w$ o; @ A: s/ bsilicon dioxide3 i( J/ ^5 T. k& Y3 t0 i
Not more than 2%, either singly or combined
$ x4 X' P* x8 t$ I" C/ aSee descriptions under TESTS
4 P: {; J: a5 MAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
4 t& @. p4 l; Walumina or silica.) O& [- b1 N1 V4 e/ Z3 V
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and8 ^# z& V% i/ P2 d4 ?1 L
place on a steam bath for 30 min with occasional stirring. Filter7 m/ X( T1 U0 _' G
through a Gooch crucible fitted with a glass fibre filter paper. Wash
_% u. `' i- B& swith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
1 R9 b& G' V# k& t. m( q9 Jcombined filtrate and washings to dryness, and ignite at a dull red! r! ^, b3 w6 {
heat to constant weight.
& |: P) X# c% @6 Z3 C& v2 rWater-soluble matter: i$ L. R6 T6 w
(Vol. 4)
% i$ _* y+ [3 m+ MNot more than 0.5%. g& @% a( Y- O. d' R/ ~6 Q( x: S
Proceed as directed under acid-soluble substances (above), using8 V, L6 b$ j( K0 B/ P
water in place of 0.5 N hydrochloric acid.' v/ j. _7 P) u0 O3 `4 l
Impurities soluble in 0.5 N! c; P0 t- j2 V' v/ o. q$ e8 x
hydrochloric acid, R) \$ x/ J$ w5 {5 e) z
Antimony Not more than 2 mg/kg
$ e7 ]7 W* d/ x9 qSee description under TESTS# C1 u6 p, P+ C+ Q* Y- g2 Z
Arsenic Not more than 1 mg/kg$ C. Z/ K9 U& x. ~
See description under TESTS9 [3 u. v7 I+ `! J' w v
Cadmium Not more than 1 mg/kg# ?, q" `1 K7 \/ n$ [" J# w* \ B
See description under TESTS% I7 W: v' ?6 K% z8 g& b, z
Lead
/ b: U6 B. y# J* B- P) \# VNot more than 10 mg/kg, L, j! ?, P6 ]4 |1 O: d$ u
See description under TESTS
/ d: ^/ X! {% U! i- gMercury (Vol. 4) Not more than 1 mg/kg
# \6 f$ b) N& n( sDetermine using the cold vapour atomic absorption technique. Select a& O8 L! X4 g7 F( }
sample size appropriate to the specified level' _7 w) ^! x7 ^$ r: x- a% l
TESTS
- y7 ~- `) \ R) p1 I& sPURITY TESTS
. k, S$ ^7 A+ ~; }Impurities soluble in 0.5 N
0 O: S! R$ }2 X5 X$ \8 M1 p+ @hydrochloric acid b, N6 q( ^9 z2 |
Antimony, arsenic,, l8 T1 t* X( ]# ?: u7 f
cadmium and lead2 P: P% g5 ~. ^0 {' j1 _5 k
(Vol.4)
+ k5 D$ q2 K& Z6 y; XTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N; l* o( `' T6 G0 |( y+ p6 N' J
hydrochloric acid, cover with a watch glass, and heat to boiling on a
- ^. d1 C \, Y8 u4 s* N- ^$ o5 _3 O5 {hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml* c. o- u$ d$ A- V) S
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
: u4 K, V. t% @9 C& y0 L/ G' Omaterial settles. Decant the supernatant extract through a Whatman. i8 ?1 x U7 E9 k5 G8 L
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
/ b! i, N$ E6 N: C2 |volumetric flask and retaining as much as possible of the undissolved. e# |$ Z% m3 F' K- I4 X" [& u
material in the centrifuge bottle. Add 10 ml of hot water to the original# s9 I& O( S& }$ z* v1 K
beaker, washing off the watch glass with the water, and pour the
9 n4 ?% Q: n+ i7 fcontents into the centrifuge bottle. Form a slurry, using a glass stirring
; B7 K0 y! X9 j+ M7 \" N8 wrod, and centrifuge. Decant through the same filter paper, and collect
2 l; w1 Y: B& c& M n mthe washings in the volumetric flask containing the initial extract.
: {7 x8 d$ P1 e/ y3 R: q. E# {- \1 wRepeat the entire washing process two more times. Finally, wash the3 l4 Q# s- R) J+ R2 h) F& z" ^
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
% ?1 }0 l% b7 oto room temperature, dilute to volume with water, and mix.* s5 s; I( |9 J [
Determine antimony, cadmium, and lead using an AAS/ICP-AES
# Y5 r$ L/ q) }: itechnique appropriate to the specified level. Determine arsenic using the1 J& n# f$ p8 E7 C% N% C; |
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using( d+ }1 y/ `* ?4 @) I
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than) f$ \, j- B3 V$ x: M9 }% Q
1 g. The selection of sample size and method of sample preparation/ n' y5 Y* U. v6 _/ e6 P4 K" J$ {8 n
may be based on the principles of the methods described in Volume 4.
9 Y4 m7 v) o W# ^& x# K, K& [+ v. EAluminium oxide Reagents and sample solutions
# e: Q! q; L, B' i0.01 N Zinc Sulfate# _8 J& }, x' a2 v" A7 f
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
' c/ C' o! ]! x, b" _1 ]$ G3 `4 ^% Jmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg) C! u" M4 m4 z' W
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of) ^8 k( F! a9 D' M( ^
concentrated hydrochloric acid, heating gently to effect solution, then
. a& J# m4 G l( ^* n, _( l9 p) Mtransfer the solution into a 1000-ml volumetric flask, dilute to volume
. Y$ x$ Z! v! _* ]& f. ewith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
. _+ R4 ]8 W* x$ F8 yml Erlenmeyer flask containing 90 ml of water and 3 ml of' }7 w/ _. H j/ z! v0 |
concentrated hydrochloric acid, add 1 drop of methyl orange TS and v6 Q: }- W) ~0 S2 b
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,( v0 J5 C) ^+ Q2 u1 ?, x5 v% y F
dropwise, ammonia solution (1 in 5) until the colour is just completely
5 i9 p L6 p% l# E7 m: y* ~, A3 S: ychanged from red to orange-yellow. Then, add:% T$ v f- K' [3 n
(a): 10 ml of ammonium acetate buffer solution (77 g of
6 }. Y" D) }( g9 G; Tammonium acetate plus 10 ml of glacial acetic acid, dilute to9 p6 |$ \3 V2 p8 i3 D( c
1000 ml with water) and
1 J: c6 G V. L6 i(b): 10 ml of diammonium hydrogen phosphate solution (150 g
; [) x9 {- i3 h* Yof diammonium hydrogen phosphate in 700 ml of water,
' w m6 l! T+ madjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
: _- N7 v5 H0 x) J5 n; _then dilute to 1000 ml with water).
7 d' [& f6 D. h2 w5 LBoil the solution for 5 min, cool it quickly to room temperature in a
& ?8 k1 _- M0 i" k: Y; X T5 kstream of running water, add 3 drops of xylenol orange TS, and mix.: y* v c1 W! Y
Using the zinc sulfate solution as titrant, titrate the solution to the first
2 r+ Y( s% p& O3 n( h6 gyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
( j1 u! X& u1 X" N2 h B6 b. n9 `This titration should be performed quickly near the end-point by
" |. X3 p- N2 M- f8 @/ x6 Iadding rapidly 0.2 ml increments of the titrant until the first colour
+ v! W- _7 Y( @' B0 q, `; kchange occurs; although the colour will fade in 5-10 sec, it is the true
; w& {, }4 `0 C. M+ \end-point. Failure to observe the first colour change will result in an1 k& C% N) A: U" c# B6 A
incorrect titration. The fading end-point does not occur at the second
" l7 S; V+ r# l$ x4 E) cend-point.)
" a# q* O( {. f9 q! n. uAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a) q4 O! w5 @: e, o" H, i' j2 B
stream of running water. Titrate this solution, using the zinc sulfate
' A/ m9 G. {" Y7 msolution as titrant, to the same fugitive yellow-brown or pink end-point+ B0 Z$ Q3 C0 i, B' `( L
as described above.
2 d$ J) U5 Y0 P9 fCalculate the titre T of zinc sulfate solution by the formula:
7 K6 R* y' m# @% G NT = 18.896 W / V
0 a8 I% @6 `6 R1 [1 xwhere% X* C H; I8 J3 m( C
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution9 x0 N7 i: M. u. Q7 L% U
W is the mass (g) of aluminium wire
7 g5 l! B M m1 L) ]% TV is the ml of the zinc sulfate solution consumed in the' ~2 L7 g: {+ u- b" F& R
second titration4 O" _* U2 T5 @
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
$ h& t7 U1 Z! C/ P: _R is the ratio of the formula weight of aluminium oxide to5 c4 C1 a; b8 l7 v8 @ |- t
that of elemental aluminium.
: q# `9 e$ Y( j2 xSample Solution A
6 t Z$ o z2 G2 q# \5 [# ?9 TAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica, b8 ^* a/ D. s6 x+ ]8 z0 t' F; N
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O). T; J/ o" P: n3 p+ Y3 @1 b
(Note: Do not use more sodium bisulfate than specified, as an excess6 K6 `9 p# f0 c
concentration of salt will interfere with the EDTA titration later on in the `7 m. H+ }, x
procedure.) Begin heating the flask at low heat on a hot plate, and$ w2 I/ O4 N# ?5 X h
then gradually raise the temperature until full heat is reached.6 b0 {3 R' y- _0 M+ Y3 k( j# h: C
(Caution: perform this procedure in a well ventilated area. ) When
/ \; f) e0 T: {) Ispattering has stopped and light fumes of SO3 appear, heat in the full
1 _+ R9 P1 }: U. E: ^9 t$ a$ R/ rflame of a Meeker burner, with the flask tilted so that the fusion of the: f8 Y( B7 S8 y
sample and sodium bisulfate is concentrated at one end of the flask.$ W; N, H5 ~, S. G
Swirl constantly until the melt is clear (except for silica content), but% S0 }: A) M! I+ R1 e* }1 a% f0 M
guard against prolonged heating to avoid precipitation of titanium
. W' N& }; Q2 y* j/ a! B: g6 ^dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
2 n( J. G2 [, b8 q$ `$ s: k( othe mass has dissolved and a clear solution results. Cool, and dilute to+ |% p9 f7 F; W, Z0 M
120 ml with water. Introduce a magnetic stir bar into the flask.
& F# `7 {9 F+ V% `7 ~3 H, G) GSample Solution B, ?3 \. G, O8 ?2 v7 h7 D: V4 g
Prepare 200 ml of an approximately 6.25 M solution of sodium
. a" N1 }$ E. b% Jhydroxide. Add 65 ml of this solution to Sample Solution A, while
4 z8 }' |# e) ]stirring with the magnetic stirrer; pour the remaining 135 ml of the# I9 ^7 U6 d) N( j
alkali solution into a 500-ml volumetric flask.' f7 g( v. }1 `( C7 p2 Y
Slowly, with constant stirring, add the sample mixture to the alkali
7 T! y$ b. X) `: H H# gsolution in the 500-ml volumetric flask; dilute to volume with water,
1 [% O7 Y9 d4 cand mix. (Note: If the procedure is delayed at this point for more than
4 n% W4 i u: c" P/ z, [2 hours, store the contents of the volumetric flask in a polyethylene8 h' t* W/ c; q* y/ q
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
& A; K7 {/ `9 k0 y4 bthen filter the supernatant liquid through a very fine filter paper. Label% U; Z, w ]5 r
the filtrate Sample Solution B." b& Z* z# V+ A5 ~) X! u1 i
Sample Solution C( u5 K" }: t$ w. R5 L. R4 B
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer" ]" E( \6 }# ^$ W, W! |
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid' k; D- Y9 P9 }9 A
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
( D' |3 C$ s- X, \6 e6 b# ]M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is4 ]) P5 @7 {* m9 g; N; A
known, calculate the optimum volume of EDTA solution to be added
, H7 O2 k1 Q5 {; i8 cby the formula: (4 x % Al2O3) + 5.]( n/ K* z( F: q9 T% A9 w. @
Add, dropwise, ammonia solution (1 in 5) until the colour is just4 p8 b1 C# h" d" |* M8 Z
completely changed from red to orange-yellow. Then add10 ml each6 [/ Z: m2 v: {, t
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to* B% N6 I8 `) L" J0 a, J+ x% C [
room temperature in a stream of running water, add 3 drops of xylenol
2 }! l) J" x; d: Iorange TS, and mix. If the solution is purple, yellow-brown, or pink,& r* i5 X# J: N7 `# V/ j" h
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired$ [7 ^/ p/ j/ U# P3 S8 z* L8 ?
pH, a pink colour indicates that not enough of the EDTA solution has- g/ |- o9 n+ y% e" x
been added, in which case, discard the solution and repeat this
3 T. J" I3 L6 f' @procedure with another 100 ml of Sample Solution B, using 50 ml,1 f7 D: n9 m5 @. t" A/ W2 b
rather than 25 ml, of 0.02 M disodium EDTA.' j9 d5 b3 t/ |
Procedure
- j8 T8 L# B9 Q$ m* K5 p9 IUsing the standardized zinc sulfate solution as titrant, titrate Sample
5 Q$ J: x. q/ P) \Solution C to the first yellow-brown or pink end-point that persists for# ~( G4 V8 }. W$ W) U
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first1 E; J5 d5 o3 n) @7 t
titration should require more than 8 ml of titrant, but for more accurate3 `) u/ k* q/ @4 c/ A) p
work a titration of 10-15 ml is desirable.0 z. H3 y0 y# N9 i* J% ~6 Q% p
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-54 v; T" S0 q' T/ i& y# Q: r9 M8 K
min, and cool in a stream of running water. Titrate this solution, using
4 p* r7 w% _! c; J3 i ythe standardized zinc sulfate solution as titrant, to the same fugitive; E' \8 ]; F$ @! u
yellow-brown or pink end-point as described above.4 S" q' R- Q- q3 [9 S
Calculation:' z: i0 F# @% R8 P1 C9 W' j
Calculate the percentage of aluminium oxide (Al2O3) in the sample
& t8 C# V& p4 z% b+ Utaken by the formula:: P" q! G; F6 a% @& y5 X
% Al2O3 = 100 × (0.005VT)/S
' `% L; _) v- p$ ?$ r2 cwhere
& H( S+ `0 \ F- S" XV is the number of ml of 0.01 N zinc sulfate consumed in
1 x5 `/ _8 h$ q. s( Q# xthe second titration,
+ I* T+ t/ Z7 ]) V- n& x1 kT is the titre of the zinc sulfate solution,1 b b+ Y! {" y2 p" Z
S is the mass (g) of the sample taken, and q, r& [8 B/ \
0.005 = 500 ml / (1000mg/g × 100 ml).& q3 _+ E4 U& w7 z$ D% n) s
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica1 j0 ~2 y* w8 A7 K" d f
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).2 `0 R `7 R7 ~# D6 f- h( ]; U w
Heat gently over a Meeker burner, while swirling the flask, until* S) Q3 A" o7 q6 J O
decomposition and fusion are complete and the melt is clear, except, p4 I4 w4 X% v$ S5 p8 S' R
for the silica content, and then cool. (Caution: Do not overheat the
0 {4 M4 Q! R* e- wcontents of the flask at the beginning, and heat cautiously during$ S( L2 g O: B# o+ V! p% B
fusion to avoid spattering.)
$ `* h% @% j2 ]) b6 J* DTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat! w) f; T3 J' T' P8 j
carefully and slowly until the melt is dissolved. Cool, and carefully add/ v7 \$ z$ F" x2 i7 h8 ~: z1 ^- \3 _9 b H
150 ml of water by pouring very small portions down the sides of the
5 W; s' e% N2 G9 A+ Hflask, with frequent swirling to avoid over-heating and spattering. Allow
% d* s, d( L# ^' \0 _) w7 athe contents of the flask to cool, and filter through fine ashless filter/ D2 a& q1 i+ e
paper, using a 60 degree gravity funnel. Rinse out all the silica from
4 @& `2 d9 Q" ^) k$ Q" x- l7 L- }& [the flask onto the filter paper with sulfuric acid solution (1 in 10).
4 t. e4 M( H4 o2 dTransfer the filter paper and its contents into a platinum crucible, dry in
' F f8 I) Q6 X9 C$ Q" xan oven at 1200, and heat the partly covered crucible over a Bunsen
' R! c i( z5 O: l% h* [burner. To prevent flaming of the filter paper, first heat the cover from
/ Q) Q: b5 t" K/ L5 v" Kabove, and then the crucible from below.: C0 ?- }, v; Q6 ^) Q; {
When the filter paper is consumed, transfer the crucible to a muffle
+ Q3 u1 [0 e/ o, e* `$ u. Lfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
8 g' \7 F6 A& W! Iweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
+ J& f: F$ M3 H+ {7 _hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
3 s1 a% N( s" u4 von a low-heat hot plate (to remove the HF) and then over a Bunsen8 [+ C$ H' Y. i5 b6 t
burner (to remove the H2SO4). Take precautions to avoid spattering,( k* e9 x" @! l b% k2 G
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a+ b B# N" b) Z1 s6 T+ r9 ~
desiccator, and weigh again. Record the difference between the two' S5 [' X( Z3 `1 }! [2 S
weights as the content of SiO2 in the sample.4 q. X/ {$ U- X8 M; O. t$ D
METHOD OF ASSAY
# X J* a; l; XAccurately weigh about 150 mg of the sample, previously dried at 105o
+ w( ?) {$ I- U" xfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water3 c! Z6 u' E& ?" @5 I; ]* B
and shake until a homogeneous, milky suspension is obtained. Add 30
5 T( ~" \" r1 H% c( ]# tml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially/ }! g5 w! S4 k/ x; t/ N" i
heat gently, then heat strongly until a clear solution is obtained. Cool,' e/ _$ L' f3 Z' ?
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
: C8 V: b+ E9 K, X2 \4 T* o3 _7 {acid, and stir. Add 3 g of aluminium metal, and immediately insert a
9 b+ x9 m9 n8 c6 U. Zrubber stopper fitted with a U-shaped glass tube while immersing the
; w+ a/ P7 H) pother end of the U-tube into a saturated solution of sodium
; r# G9 n9 m4 C& ]9 f% Gbicarbonate contained in a 500-ml wide-mouth bottle, and generate, W. N& R* s7 c1 d- H. a3 b4 P
hydrogen. Allow to stand for a few minutes after the aluminium metal
0 W% k0 u( K/ c4 f1 }has dissolved completely to produce a transparent purple solution., I6 C6 q- s. d8 U) q: @/ W* p
Cool to below 50o in running water, and remove the rubber stopper- H) ?8 r; v' Y3 \5 ^$ G$ K
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate6 x7 R0 C8 l( Z8 c. y+ {8 G8 U
solution as an indicator, and immediately titrate with 0.2 N ferric9 P# z5 I( n4 }" B. S0 a
ammonium sulfate until a faint brown colour that persists for 30; t; ~* T3 t+ ^& [! }& l5 e9 `
seconds is obtained. Perform a blank determination and make any6 G8 u) M: L: J# b* w) r
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
# o2 j' Z* J6 l- ` y" ?equivalent to 7.990 mg of TiO2.
6 b5 {+ D( p$ ]2 b. } |
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