|
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): v" P, o0 G/ N" u) J
! V: U4 j: A( wJECFA关于二氧化钛(钛白粉)的结论% {2 T4 H* H. c" w6 J
* I. s& H; L" w% i* ]% G" d
摘要: 2006年JECFA关于二氧化钛的结论1 m( C8 _" S& `$ b% V
ADI值:不作限制。
8 Q e5 c' K F# E3 {) x功能:着色剂
, I0 P' \# N z3 T+ s
7 P+ X. S& M: [8 X' h L8 b+ NTITANIUM DIOXIDE4 M* W6 n7 D4 R. r Q. [8 i
Prepared at the 67th JECFA (2006) and published in FAO JECFA1 G' c0 a8 X8 C/ a; L
Monographs 3 (2006), superseding specifications prepared at the 63rd
9 t: u0 [% n' i+ G" d) n. |) `JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
/ E5 t' R# x4 I( c' i( j6 @' [6 x/ zCombined Compendium of Food Additive Specifications, FAO JECFA4 x" G; o, @% i2 n
Monographs 1 (2005). An ADI “not limited” was established at the 13th
- e9 t3 M6 r7 q \+ EJECFA (1969).* a; @0 W, Q: _
SYNONYMS$ I" j5 g: a: a0 v
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
. A8 P1 O# n5 j0 X" {" \DEFINITION
2 @, s4 X m2 ~ |; ~& U6 f% TTitanium dioxide is produced by either the sulfate or the chloride
5 H( w% C3 z+ |% hprocess. Processing conditions determine the form (anatase or rutile
8 i8 v0 g/ e5 X5 z" ?/ y0 ~& Dstructure) of the final product.0 A& }. Y! \" e
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)- J7 F l4 D8 }- B/ b: s( d
or ilmenite and titanium slag. After a series of purification steps, the0 H* E w( M; @- W$ j+ G6 @& |0 U' P) }
isolated titanium dioxide is finally washed with water, calcined, and
4 X6 h+ Z+ W+ j o0 f$ J9 a1 F7 pmicronized.
- r) z$ O& Y7 o' A3 ?In the chloride process, chlorine gas is reacted with a titaniumcontaining
6 O' f2 z( T2 B9 f) {! Lmineral under reducing conditions to form anhydrous) C+ G# B+ J6 d; C
titanium tetrachloride, which is subsequently purified and converted to# I: u C9 x; H w7 H" M2 o
titanium dioxide either by direct thermal oxidation or by reaction with" t' w5 U3 ?) C% x6 l& G
steam in the vapour phase. Alternatively, concentrated hydrochloric
- W% F h& N M4 w- j' Vacid can be reacted with the titanium-containing mineral to form a2 @9 v5 `% e3 p0 V0 O* U
solution of titanium tetrachloride, which is then further purified and; C8 P' _3 g1 e# N$ h; N
converted to titanium dioxide by hydrolysis. The titanium dioxide is8 W' b# `5 c3 o8 I- Q6 ? {
filtered, washed, and calcined.
1 I) X9 ^% {. V3 ZCommercial titanium dioxide may be coated with small amounts of
/ ~" o! u( y! Z) _' Halumina and/or silica to improve the technological properties of the
. {0 U- n9 ]; w1 G# jproduct.
/ Z5 l9 G Q1 FC.A.S. number 13463-67-7
8 ^* l. c; x% H& dChemical formula TiO2/ B8 x8 N, S9 @: B2 L
Formula weight& o$ L' l& H0 R( V/ {3 E
79.88
5 l( G1 i7 o& u2 K1 pAssay
( y8 b! Z; W3 C) x# Y! A: Q" H" VNot less than 99.0% on the dried basis (on an aluminium oxide and
# `# {$ ?+ l" d G! I8 |silicon dioxide-free basis)
3 z9 \9 b8 n' J. F# O6 S5 H$ N8 S2 iDESCRIPTION
. R J4 |: b7 a& o5 I/ pWhite to slightly coloured powder
3 W' |6 N; m. P( ]; u$ `! T2 V6 s5 wFUNCTIONAL USES0 L9 p* W& ?; v" L+ |/ I# h5 X/ T
Colour
( n& Y) ^3 ^: w1 k% d2 ]CHARACTERISTICS; y; m+ N7 u7 K3 {1 w: S9 u" @
IDENTIFICATION
+ W$ u& q' i/ L: ^) iSolubility (Vol. 4)1 o# m8 C( t. P6 ^2 y4 @
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
% v" S0 o" D7 n2 c4 l7 \solvents. Dissolves slowly in hydrofluoric acid and hot concentrated) p+ b1 e/ a; p2 z
sulfuric acid.) U- |7 [# C/ N$ X: |+ G
Colour reaction. v4 {; z4 {9 |& A2 S
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
+ _" V$ ]* T" M! w( _: I1 a& r0 v6 jsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with; T3 h" T! n4 ~
water and filter. To 5 ml of this clear filtrate, add a few drops of- X$ r" K S0 _, J8 J, x' S
hydrogen peroxide; an orange-red colour appears immediately.
2 G; q% z0 X9 G! sPURITY. b" @6 Z) |7 r
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)3 x7 `, I4 v# Y
Loss on ignition (Vol. 4)
$ A$ o; H8 g& r; \2 U# {Not more than 1.0% (800o) on the dried basis
! }+ |/ @6 t4 Z6 L1 TAluminium oxide and/or
2 H& L5 r( s2 V9 ]# F/ `) G0 osilicon dioxide. N- U( d7 [" f/ q5 M
Not more than 2%, either singly or combined
, }( i: y3 E" l4 ^ TSee descriptions under TESTS. Y; M4 q9 X4 m @: \
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
' L6 K- F' D- I2 \' }0 Q- I0 Oalumina or silica.8 O2 g [7 @; k/ e
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
/ [% a. \; @$ O5 ^6 A `place on a steam bath for 30 min with occasional stirring. Filter
$ S" ~; Z2 I9 l8 rthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
/ H( y; K" r8 Vwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the. m$ O; r/ E! y/ `# @
combined filtrate and washings to dryness, and ignite at a dull red4 Z6 N' a6 [: R3 k* {
heat to constant weight.
$ Y2 f$ I& }/ D& b* E9 bWater-soluble matter0 r3 Q& Y) H Z6 [8 g5 \
(Vol. 4)4 y0 D* {1 {4 e. B+ s
Not more than 0.5%
+ j8 D8 ]( M' j! ?% lProceed as directed under acid-soluble substances (above), using% R3 h: \7 }( z0 ` G' o. h
water in place of 0.5 N hydrochloric acid.
3 r# J4 c2 p; j6 F: dImpurities soluble in 0.5 N+ y# [: W0 ?- J
hydrochloric acid: ]/ e* s/ g! |" I7 k. F
Antimony Not more than 2 mg/kg! t3 E9 W9 j5 W& _
See description under TESTS
3 [& F m. n3 u. f( L0 n+ ?. XArsenic Not more than 1 mg/kg
" m6 @+ m/ E0 @- B, ^) c; u( r0 _0 `See description under TESTS8 U5 `0 V/ ~2 w+ V# {! |
Cadmium Not more than 1 mg/kg6 z% o5 _5 G7 D1 }" V4 g, w R6 _
See description under TESTS
! O q8 _' n5 ? t/ K* vLead
, M' A" Q1 y% S( J9 H, j! T7 NNot more than 10 mg/kg0 }6 E' |6 ?3 I" ]
See description under TESTS
8 s. L! w' t- vMercury (Vol. 4) Not more than 1 mg/kg& L$ l9 @1 ]2 y$ x# \9 V9 X
Determine using the cold vapour atomic absorption technique. Select a! _2 ]; X, w; O7 o' D# g5 c. q
sample size appropriate to the specified level0 t- M5 y* g) n- a7 r2 p" a
TESTS
7 Z5 \4 g5 \' W: r: r4 G& |+ kPURITY TESTS
) I2 s3 ^. I$ ?/ b$ @- [9 dImpurities soluble in 0.5 N
0 _- s6 [( f5 d4 J; Lhydrochloric acid
1 H7 {, u& q& U% |- y- W$ E! YAntimony, arsenic,
+ R5 V+ k1 A& P8 \$ Lcadmium and lead
+ k& X' X) a6 N/ |% C- d( e(Vol.4)
) S& F; d! q4 o3 n/ BTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N0 F/ k8 R$ d" t4 ~* b- [' S) N
hydrochloric acid, cover with a watch glass, and heat to boiling on a3 \7 `5 f1 J$ w* X& q6 |. |- Q
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml# w- }: {# N0 W( E3 K% `5 W& Z
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved, ?" K/ ]1 b# G) o |6 q5 }
material settles. Decant the supernatant extract through a Whatman
& u+ z. d0 A3 N' R# a lNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
( x! p* D) r* ^; vvolumetric flask and retaining as much as possible of the undissolved% t. p# \# n+ J" }2 p" I
material in the centrifuge bottle. Add 10 ml of hot water to the original
. |8 s- M! F& g3 P$ I& K3 nbeaker, washing off the watch glass with the water, and pour the! z3 w0 C: {3 p+ U7 f" w. \
contents into the centrifuge bottle. Form a slurry, using a glass stirring- A |2 ~9 B* B1 D4 {& O. z
rod, and centrifuge. Decant through the same filter paper, and collect! _/ M! K9 j; G, ?; [/ ?* }$ I
the washings in the volumetric flask containing the initial extract.
+ }& B) d: a* L7 A+ t. b5 T+ ERepeat the entire washing process two more times. Finally, wash the
6 a8 d( I6 W) _' t0 ffilter paper with 10 to 15 ml of hot water. Cool the contents of the flask6 j* ^, ~ M7 p) [+ E* D7 A' Q9 G5 q. Z
to room temperature, dilute to volume with water, and mix.
/ G; R1 X I UDetermine antimony, cadmium, and lead using an AAS/ICP-AES
6 X: C0 I5 f" _2 C" O8 S/ q+ n9 ztechnique appropriate to the specified level. Determine arsenic using the
+ r% w' C8 N1 I. q+ MICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
0 G! Y& W5 ]' u. IMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
, K) ^6 y/ S- h p1 g. The selection of sample size and method of sample preparation
+ q! w7 A. @5 H2 @, ~& M2 hmay be based on the principles of the methods described in Volume 4.
% x- E1 z, f; ~' yAluminium oxide Reagents and sample solutions; j; k1 O1 H1 @5 \
0.01 N Zinc Sulfate
$ P, z0 Q. H" i7 w! _6 p! gDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to7 u t) j( m& k- C
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg* }2 m4 K' b- }; f6 ]
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of ^6 \" J; Q7 q
concentrated hydrochloric acid, heating gently to effect solution, then
' I! ?* P1 Y% u) \( {transfer the solution into a 1000-ml volumetric flask, dilute to volume
" E/ k3 ]( p& R' `with water, and mix. Transfer a 10 ml aliquot of this solution into a 500% |4 j9 z0 w) p$ l0 f
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
* t% p# k5 e: V5 G/ Jconcentrated hydrochloric acid, add 1 drop of methyl orange TS and, ~/ b7 P3 C" H: R$ c/ r
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
) E! x5 u7 j3 n) |4 G( Zdropwise, ammonia solution (1 in 5) until the colour is just completely: P: Z: z2 B+ W2 k2 b9 ^( F4 ?! C
changed from red to orange-yellow. Then, add:" s8 F0 C3 ?( h! c; r. R0 F+ y- v
(a): 10 ml of ammonium acetate buffer solution (77 g of
7 G: h# i; h* q/ n, j" _% Oammonium acetate plus 10 ml of glacial acetic acid, dilute to G5 `/ U2 v% y2 \
1000 ml with water) and
. z8 b' e7 j3 }0 P, P* l(b): 10 ml of diammonium hydrogen phosphate solution (150 g
/ E( Z. q- B: T O# wof diammonium hydrogen phosphate in 700 ml of water,6 C }9 T l w* o2 _
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
/ i9 y+ \8 }7 O$ j. t( m+ p: q: }then dilute to 1000 ml with water).1 E) p+ Y n8 F( U' C c- z( }
Boil the solution for 5 min, cool it quickly to room temperature in a- g/ u; Z: a- r+ G! E$ X5 @( u! D
stream of running water, add 3 drops of xylenol orange TS, and mix.
8 \: D: U5 O2 x; rUsing the zinc sulfate solution as titrant, titrate the solution to the first
7 E& i W' u7 o wyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:' q" i: O/ ?8 S& K
This titration should be performed quickly near the end-point by
5 ?6 s$ C9 R! U2 X9 r8 {adding rapidly 0.2 ml increments of the titrant until the first colour
+ J& q, V. C4 `change occurs; although the colour will fade in 5-10 sec, it is the true
1 I: L) {# W6 @0 c: |7 Qend-point. Failure to observe the first colour change will result in an
7 ?- d( a: v6 ^. O( b7 L: W4 uincorrect titration. The fading end-point does not occur at the second
3 s; E" k3 `) N" w1 U5 Send-point.)
' j5 z! y# z2 P- q+ s+ MAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
3 f" d9 x2 @" ~stream of running water. Titrate this solution, using the zinc sulfate
7 C( z1 n' L! o/ z0 o4 J( u, gsolution as titrant, to the same fugitive yellow-brown or pink end-point
' q- Z( u* X3 h& T3 b* L/ M3 {4 Mas described above." I! I4 q; U- H; \6 l
Calculate the titre T of zinc sulfate solution by the formula:+ e3 \' m: \% J) h
T = 18.896 W / V( Q. y5 H3 T9 w% K9 I$ ~1 X, P `
where0 q- q0 B1 g0 S( G r( O, T
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution* U' W! m1 t5 }, M* W
W is the mass (g) of aluminium wire3 m# f/ {+ s u# i+ V6 O# w- M
V is the ml of the zinc sulfate solution consumed in the+ _+ X7 n% K) ^- D
second titration
' P) K S- p8 z' i! q7 B18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
# w J3 n: a+ ~& D wR is the ratio of the formula weight of aluminium oxide to2 F2 u+ y- z' D
that of elemental aluminium. _' H& X: j! @2 T+ R# {$ I
Sample Solution A) u& z; ]3 p" ]5 j6 q% ^
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica+ {# c6 h/ p* Y$ Y5 f$ g# @& j; H
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
4 d" k- W" T' w(Note: Do not use more sodium bisulfate than specified, as an excess T3 Z: @8 G3 U+ v- u9 B: ?, K
concentration of salt will interfere with the EDTA titration later on in the
- u+ T4 q! O9 u# H1 q) Bprocedure.) Begin heating the flask at low heat on a hot plate, and% b# s0 E* |: ]$ q- r
then gradually raise the temperature until full heat is reached.0 f* F' L' m8 ?7 v6 N
(Caution: perform this procedure in a well ventilated area. ) When) M8 ?- }6 ~- x- y% U& S
spattering has stopped and light fumes of SO3 appear, heat in the full
! ^6 J5 Z0 J/ w$ N1 @' R( v, jflame of a Meeker burner, with the flask tilted so that the fusion of the: A4 U% j1 I) G
sample and sodium bisulfate is concentrated at one end of the flask.( d1 J% ?/ {, B0 H0 h/ P
Swirl constantly until the melt is clear (except for silica content), but
& F/ @! ?; [- w6 a) z3 R5 r& qguard against prolonged heating to avoid precipitation of titanium
0 T; D$ O+ I2 d. x# \0 F# ddioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
3 m( e- H5 e; F$ F, T7 a H, U( [the mass has dissolved and a clear solution results. Cool, and dilute to. @/ i/ a& _4 e9 R3 y
120 ml with water. Introduce a magnetic stir bar into the flask.
3 u# M* C* h) D* g! k" M* {8 pSample Solution B
, x7 K# O! X s1 fPrepare 200 ml of an approximately 6.25 M solution of sodium! D V& A' J% `' R9 p1 f5 X
hydroxide. Add 65 ml of this solution to Sample Solution A, while# F/ U9 p& S# n! t7 K
stirring with the magnetic stirrer; pour the remaining 135 ml of the3 ~( F8 r1 F: u# ?; r2 E6 _
alkali solution into a 500-ml volumetric flask.
, C% _+ w- |: n7 }Slowly, with constant stirring, add the sample mixture to the alkali9 {9 @6 n0 C/ \0 @
solution in the 500-ml volumetric flask; dilute to volume with water,/ J G/ @) s) b0 O D4 |: c
and mix. (Note: If the procedure is delayed at this point for more than
2 H& p/ n$ w3 T# y5 K' e2 hours, store the contents of the volumetric flask in a polyethylene# v) I. }! ^6 l) t& f" c
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
6 f" O( g/ Z- k% ^' ]$ wthen filter the supernatant liquid through a very fine filter paper. Label
1 D0 h0 t1 I# M$ j* k4 r- ~8 Tthe filtrate Sample Solution B." ?( Z" Y# Q8 ~) Q/ }( l0 Z: k" j- I3 X$ T
Sample Solution C
q: {. T: @) @0 r% C" ATransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
9 r3 B1 o7 v/ v# r2 N. D2 I1 fflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid+ U( x9 h @5 s( d3 M
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.022 v0 h( t6 ~+ D+ ]
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is. ^% P( J3 ?8 [6 k( s+ L
known, calculate the optimum volume of EDTA solution to be added
# n$ \$ l8 D0 P* Q' `6 a7 uby the formula: (4 x % Al2O3) + 5.]
2 K4 D" v& p3 d5 ~5 IAdd, dropwise, ammonia solution (1 in 5) until the colour is just
# o7 u( k& k3 l9 O, z' zcompletely changed from red to orange-yellow. Then add10 ml each
* v8 F; T' X+ Wof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
" H$ s! t3 P0 i6 Y$ p0 f! L/ m Troom temperature in a stream of running water, add 3 drops of xylenol
" \1 M# X, U4 s5 d8 J1 m6 _! ~* forange TS, and mix. If the solution is purple, yellow-brown, or pink,
5 L7 G5 @1 e4 Y, d4 @+ j# u& H+ obring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
2 S6 T$ p2 g2 |/ S8 {pH, a pink colour indicates that not enough of the EDTA solution has
4 l: A. ~ Q/ lbeen added, in which case, discard the solution and repeat this
8 ^- a I: V: m2 y5 m: ^procedure with another 100 ml of Sample Solution B, using 50 ml,
Q+ i1 S. b( D, w) |6 krather than 25 ml, of 0.02 M disodium EDTA.% k$ E! \! R4 ` b! {, H& D
Procedure" `4 r/ R- g" V) ?7 G
Using the standardized zinc sulfate solution as titrant, titrate Sample* [' Y" c5 @! [( X' E9 E' k
Solution C to the first yellow-brown or pink end-point that persists for
" i) {$ v. u- y5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
j. p0 j0 V+ ?4 j% Dtitration should require more than 8 ml of titrant, but for more accurate$ \, Y( h4 s( Z
work a titration of 10-15 ml is desirable./ F& H3 S# \" U9 `
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
9 A+ S9 \) j6 U( Kmin, and cool in a stream of running water. Titrate this solution, using
6 {6 a i% j, dthe standardized zinc sulfate solution as titrant, to the same fugitive' t6 F: W( u1 t# H: ?9 m2 J
yellow-brown or pink end-point as described above.8 W( a& U" D6 I( v4 z
Calculation:
$ q4 k( C9 v2 U3 SCalculate the percentage of aluminium oxide (Al2O3) in the sample
9 v" \' V# Y6 U) P) otaken by the formula:) {/ H x, G: ~! H7 @- e
% Al2O3 = 100 × (0.005VT)/S
2 z' c- [' G2 H' E$ qwhere
( Q5 d( H& j' DV is the number of ml of 0.01 N zinc sulfate consumed in. u) M; J# i4 r; C
the second titration,
4 I1 n+ ?0 M3 B+ H5 a1 j/ b# d% |T is the titre of the zinc sulfate solution,
5 b1 a1 J O) F2 | W+ j' [( P gS is the mass (g) of the sample taken, and( ~3 c! F& n$ c+ x; G. o
0.005 = 500 ml / (1000mg/g × 100 ml).1 F: \$ ^ K; l( O) t8 B, W4 V
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica( C/ N* L0 H3 Z6 t4 ]) x k% d
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).3 a2 g; F1 r6 F1 S
Heat gently over a Meeker burner, while swirling the flask, until% A0 `0 U5 [* v5 t- F
decomposition and fusion are complete and the melt is clear, except
( D" V" O6 v- o f+ c9 @for the silica content, and then cool. (Caution: Do not overheat the
% a) p& k0 Q2 t1 ]contents of the flask at the beginning, and heat cautiously during$ l7 P" r3 F& `$ i* V
fusion to avoid spattering.)$ a3 P6 P2 u4 a( j9 P) N
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat- G0 e% I5 [) ^$ K9 t; P, \# X
carefully and slowly until the melt is dissolved. Cool, and carefully add" j2 A9 W* Q" |: M! p
150 ml of water by pouring very small portions down the sides of the
1 J: F2 g4 j |% gflask, with frequent swirling to avoid over-heating and spattering. Allow
; C3 B# k# j% U8 Ethe contents of the flask to cool, and filter through fine ashless filter; J: k M/ ~/ W& x( [8 C8 w) u& n
paper, using a 60 degree gravity funnel. Rinse out all the silica from1 d1 Z1 }5 \$ @* ~2 O) D& K+ q
the flask onto the filter paper with sulfuric acid solution (1 in 10).6 Y, h; V1 J$ z; g& z. `& l& k7 }
Transfer the filter paper and its contents into a platinum crucible, dry in
) N/ p" g, O6 _# aan oven at 1200, and heat the partly covered crucible over a Bunsen
1 j; s) \" h2 S8 F6 N' a& _1 Y% dburner. To prevent flaming of the filter paper, first heat the cover from4 F% K% H0 B ^0 F! {
above, and then the crucible from below.
; }- U$ N3 k8 {$ Z9 D/ H, L& rWhen the filter paper is consumed, transfer the crucible to a muffle+ F6 _* ^4 d8 H& y( e
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
& }; [" `2 X" w x* D7 ]weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated( v: `* G# f4 [5 s: w& |7 {) P
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first. |( M1 `# w. P3 D1 O$ M
on a low-heat hot plate (to remove the HF) and then over a Bunsen
8 H. b" R" X6 C' z2 I. Uburner (to remove the H2SO4). Take precautions to avoid spattering,
+ k, X& x; W3 jespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a. K5 \3 m9 O. O) n' d7 u
desiccator, and weigh again. Record the difference between the two& e9 ~7 t# Y) i
weights as the content of SiO2 in the sample.
/ \) \5 F# N: U8 m5 ~METHOD OF ASSAY
6 d a: S5 ~4 UAccurately weigh about 150 mg of the sample, previously dried at 105o+ h; E4 j2 L5 v
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
; k/ Q# [$ M6 Z% _and shake until a homogeneous, milky suspension is obtained. Add 30
$ H: p! d( u; xml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
; y* {6 B2 W$ j4 u A3 Nheat gently, then heat strongly until a clear solution is obtained. Cool,' [" d: b' h$ N: e& e3 i
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
! {# ~6 j/ N6 X6 R' q" V4 L: Racid, and stir. Add 3 g of aluminium metal, and immediately insert a$ V2 t# l8 {/ z G0 B
rubber stopper fitted with a U-shaped glass tube while immersing the
n: Q+ T* u2 I; n' h1 q5 d1 y4 u/ wother end of the U-tube into a saturated solution of sodium5 Y Y9 p( \( s; m
bicarbonate contained in a 500-ml wide-mouth bottle, and generate- ]8 a! g( _; T9 @" O, s
hydrogen. Allow to stand for a few minutes after the aluminium metal( `8 F: ]; e2 Y5 l3 }
has dissolved completely to produce a transparent purple solution.
; V2 I3 C. w( HCool to below 50o in running water, and remove the rubber stopper6 N2 a' i) O9 a! B
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
' R f2 O" A. K5 }& Dsolution as an indicator, and immediately titrate with 0.2 N ferric8 a$ K7 ^9 ~( x
ammonium sulfate until a faint brown colour that persists for 30* p! u$ {( l$ x. z8 d G
seconds is obtained. Perform a blank determination and make any9 P& l# u# b4 f" O( u
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
1 y$ Z2 ?5 i6 S5 b) k* B0 t, q/ S& }: lequivalent to 7.990 mg of TiO2.8 u) S& w4 \: X* i- T+ l- w1 f
|
|