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二氧化钛(钛白粉)

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发表于 2008-5-23 12:09:00 | 只看该作者 回帖奖励 |倒序浏览 |阅读模式
二氧化钛(钛白粉) : N: w7 Z: g  ~- K% \% ?& |
0 F* L  r7 \: w# @) t& z& I- X

" h# M9 v, t6 \. V9 R4 fCAC关于二氧化钛(钛白粉)的使用规定
! ~6 U, E; d( g: G% kGSFA Online 5 O2 \2 |. p* h1 ~! l
Food Additive Details
1 d4 S& a( x, d8 B% JTitanium Dioxide (171)/ ~2 q* c+ y; Z6 q' |. Q
Number Food Category  
) @: v' i; S. B8 a  01.1.2 Dairy-based drinks, flavoured and/or fermented (e.g., chocolate milk, cocoa, eggnog, drinking yoghurt, whey-based drinks)  & S3 b  d8 u1 p5 x
  01.3 Condensed milk and analogues (plain)  ) ]6 M. D7 h$ G' l
  01.4.3 Clotted cream (plain)  
/ W0 J6 M1 E. G! a  q  01.4.4 Cream analogues  
8 o1 v& Y" Z5 F9 O4 T6 X  R  01.5 Milk powder and cream powder and powder analogues (plain)  
2 _+ O, Y: ^; R0 f: C, k  01.6 Cheese and analogues  
5 |4 o6 ^' X0 m+ m1 |6 D' ]! W  01.7 Dairy-based desserts (e.g., pudding, fruit or flavoured yoghurt)  
# W2 I+ ~) {9 N  01.8 Whey and whey products, excluding whey cheeses  
! r9 I* Q& A- m& k1 z! W& h% P  g* I# i  02.2.1.2 Margarine and similar products   
' A$ \! q! r7 O8 Y  02.2.1.3 Blends of butter and margarine  5 E+ e5 M' e2 T: [! }
  02.2.2 Emulsions containing less than 80% fat     l% r6 a2 E& F" s& j
  02.3 Fat emulsions maily of type oil-in-water, including mixed and/or flavoured products based on fat emulsions   
* M/ _- n0 p# f% t0 X( q  02.4 Fat-based desserts excluding dairy-based dessert products of food category 01.7  
( c; Q1 |/ E1 y) F! T  Y9 h  03.0 Edible ices, including sherbet and sorbet  + a- T- Y  c* a" ^9 n. [
  04.1.2 Processed fruit  3 {- l' e4 r/ q6 F2 _1 J8 }
  04.2.2.2 Dried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweeds, and nuts and seeds  ) ~+ s/ X. J& q2 t2 V, l/ [
  04.2.2.3 Vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera) and seaweeds in vinegar, oil, brine, or soy sauce  
% ?2 C, X& f1 c% g/ T. V  04.2.2.4 Canned or bottled (pasteurized) or retort pouch vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  
2 p* v7 e' l" h  04.2.2.5 Vegetable (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweed, and nut and seed purees and spreads (e.g., peanut butter)  , N0 O& j, a/ P1 |( t0 R
  04.2.2.6 Vegetable (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweed, and nut and seed pulps and preparations (e.g., vegetable desserts and sauces, candied vegetables) other than food category 04.2.2.5  
2 c4 }; Z4 F3 m% F7 I  04.2.2.8 Cooked or fried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  ' `) |3 w% [* a/ g5 P0 `
  05.0 Confectionery  3 ~: j4 W) B/ q& b
  06.3 Breakfast cereals, including rolled oats  1 _& u2 B' N, N
  06.4.3 Pre-cooked pastas and noodles and like products  
1 Z* C. l( K/ D: h" c$ V3 [  06.5 Cereal and starch based desserts (e.g., rice pudding, tapioca pudding)  
" R, z; K; A8 _" G/ h' V" D" s  06.6 Batters (e.g., for breading or batters for fish or poultry)  
' _  F& R' _& X" C9 ]  06.7 Pre-cooked or processed rice products, including rice cakes (Oriental type only)  
' }* A, V( K7 W9 C  06.8 Soybean products (excluding soybean products of food category 12.9 and fermented soybean products of food category 12.10)  
6 a4 D3 Y/ u. x# t+ t& v$ ]: h  07.0 Bakery wares  - W) }  U/ F# l# {
  08.2 Processed meat, poultry, and game products in whole pieces or cuts  
3 K8 R8 R4 N) e8 N  08.3 Processed comminuted meat, poultry, and game products  
" ?& j7 ?. q4 O+ Y8 P  08.4 Edible casings (e.g., sausage casings)  / ?& N- T1 M% v! v% ?1 w4 K& {/ M
  09.3 Semi-preserved fish and fish products, including mollusks, crustaceans, and echinoderms  
7 Y+ j% u7 u. D) t2 i' f+ P5 j( l# w7 l  09.4 Fully preserved, including canned or fermented fish and fish products, including mollusks, crustaceans, and echinoderms  
3 R  P3 q; y' h- j  10.2.3 Dried and/or heat coagulated egg products  
. H$ ~% L4 ~1 S/ l. B( F9 @  10.3 Preserved eggs, including alkaline, salted, and canned eggs  $ g+ ^0 W& V; y+ i! z* p" A
  10.4 Egg-based desserts (e.g., custard)  
) E* ?1 H$ E7 _6 x( u: R  11.6 Table-top sweeteners, including those containing high-intensity sweeteners  % n) I  G2 l- U
  12.2.2 Seasonings and condiments  - t; [2 s: W. e4 r
  12.3 Vinegars  
7 o- B+ B% Z4 j1 }! X* q  12.4 Mustards  - o0 r* L# W) _# Q" k, |5 u
  12.5 Soups and broths  * @( M6 p: X7 n& o& X& u) U
  12.6 Sauces and like products  ) ~8 S7 j0 x, R
  12.7 Salads (e.g., macaroni salad, potato salad) and sandwich spreads excluding cocoa- and nut-based spreads of food categories 04.2.2.5 and 05.1.3  * u# e- f1 b! |! w) o
  12.8 Yeast and like products  
7 x2 N. ^' F( Q! I* w  12.9 Protein products  
( _+ b- j6 m% g+ d1 V  12.10 Fermented soybean products  : r3 q9 a& ^: a6 T9 m! l! ?+ \; R
  13.3 Dietetic foods intended for special medical purposes (excluding products of food category 13.1)  , o# o4 b9 e+ W7 k# z
  13.4 Dietetic formulae for slimming purposes and weight reduction  9 {! k( L' d; L" g, }9 L
  13.5 Dietetic foods (e.g., supplementary foods for dietary use) excluding products of food categories 13.1 - 13.4 and 13.6  
3 [2 h/ v, ^- q' m  13.6 Food supplements  
  @' I- ~; E7 @2 o  14.1.1.2 Table waters and soda waters  
  h4 G: K' f* B% [- _  14.1.4 Water-based flavoured drinks, including "sport," "energy," or "electrolyte" drinks and particulated drinks  
5 V: M- s# a7 F" t* }$ z# _7 c  14.2.1 Beer and malt beverages  
* }. Y: N) f6 Y# W: v" O; z  14.2.2 Cider and perry  $ v' c  {7 W( t" q! Z" F1 `7 _
  14.2.4 Wines (other than grape)  / l1 o8 U" ~8 c3 ^2 A
  14.2.5 Mead  ( |! n0 h. D. ?  d  F7 f; r
  14.2.6 Distilled spirituous beverages containing more than 15% alcohol  
3 t' J  C' u( T: h. X/ |  14.2.7 Aromatized alcoholic beverages (e.g., beer, wine and spirituous cooler-type beverages, low alcoholic refreshers)  / O; S$ l2 U8 r$ L$ }7 d& W
  15.0 Ready-to-eat savouries  5 o6 X( Z1 A2 [% S& t8 E
  16.0 Composite foods - foods that could not be placed in categories 01 – 15& ?+ o0 o- r( `4 D

# v+ q& h& n* Y5 d# Z
& E& L4 I* r0 ~+ K) }& L) n部分译文:$ _- e; i8 v9 d$ ^- i8 ^- R
: U4 A8 v0 S- R  M: J
食品添加剂通用规则5 R8 r: L) c9 |2 E* R2 I& X
食品添加剂
" y) u2 y1 [) A6 {                    二氧化钛(171)
3 f5 b1 M( o" g, p; v/ T* E! s' g食品类别:
# n7 |# P! ]7 Y. H$ m1 D$ W06.3 早餐谷类,包括燕麦片" y) F* `/ S! t0 h: |
06.4.3面条及类似产品& s& w2 o7 ]$ m3 j
06.5 谷类,淀粉甜点(包括:米粉布丁,木薯布丁)( q+ J  {$ ~. O. O
06.6 面团4 L; v3 V, u$ `! A
06.7 预煮的或加工的米产品,包括年糕(只包括中式的)06.8 Soybean products
& G- k% r1 W' @% \% }07.0 烘焙类3 \% x5 q, D; j9 X8 X
07.1 面包,普通烘焙类,以及其混合物
5 G8 @5 B; p' p: R: w* K+ I5 |6 h9 t07.1.1 面包,面包卷
7 L6 @5 O3 q1 |* V+ z( W- B8 _07.1.1.1 酵母发酵面包及特殊面包
& b" @( B( f2 @07.1.1.2 苏打面包( E' i+ n& g2 U# }, N+ a' e
! L; k3 d0 {1 c& Z! f+ B, [
0 c8 s5 r3 I3 Z& _2 S, A( H# g9 z1 a
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 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)6 a$ s9 g: W7 \1 O0 n

  I' z$ Q1 p% V% mJECFA关于二氧化钛(钛白粉)的结论( ~% q5 Z  {2 I' w* \

4 m$ N" ?3 D& y# r摘要: 2006年JECFA关于二氧化钛的结论* z, J& `& |+ X3 s3 g( x
ADI值:不作限制。
; b4 G* ]9 M6 y1 d功能:着色剂
$ j/ [/ R" H; m. o) x
2 E# Y& c* k- H" sTITANIUM DIOXIDE
3 U. t( U6 H; a. n1 d3 yPrepared at the 67th JECFA (2006) and published in FAO JECFA
3 q8 f3 h9 u% Y' x& J7 ]  f5 k8 d+ `Monographs 3 (2006), superseding specifications prepared at the 63rd
4 `2 l: X8 }7 D9 k, {: Q0 @* LJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
1 U8 P: A6 j, C4 `Combined Compendium of Food Additive Specifications, FAO JECFA
$ \7 I0 Z) U7 v3 N8 hMonographs 1 (2005). An ADI “not limited” was established at the 13th
2 ^2 |0 Y8 K9 N; E1 GJECFA (1969).. S  U& I8 Y' X" K" |8 ^5 e1 H
SYNONYMS& V# e+ Y/ x7 v, A0 w
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171$ X* |4 M1 [7 O* G" a+ X
DEFINITION4 O1 [& S& ~4 o) E% P- i
Titanium dioxide is produced by either the sulfate or the chloride
! M  v: e8 k! i7 G# u) L; ?process. Processing conditions determine the form (anatase or rutile
# I9 `% i3 G, C6 M0 _6 C6 F3 lstructure) of the final product.$ L* X" m. w8 N; Q
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)5 C. Z( Q6 ?8 j; V) F. n$ d
or ilmenite and titanium slag. After a series of purification steps, the) f! H+ O' H9 T1 U0 t
isolated titanium dioxide is finally washed with water, calcined, and
$ E* L& o6 F. `9 W6 A- p6 Zmicronized.
# W! |' G, k' K% n8 pIn the chloride process, chlorine gas is reacted with a titaniumcontaining
* F6 ]; {$ q8 }3 n& p+ \* p8 Bmineral under reducing conditions to form anhydrous9 H, n( i0 |' b  M
titanium tetrachloride, which is subsequently purified and converted to( C, h: g. m- Y$ g1 g; c8 K; o
titanium dioxide either by direct thermal oxidation or by reaction with
: c' N9 n: k) S$ A7 H* rsteam in the vapour phase. Alternatively, concentrated hydrochloric- Z9 B$ {# a2 c) u, a6 Z# F
acid can be reacted with the titanium-containing mineral to form a3 _; D9 j- {, s0 N8 p: g. ~- q: t
solution of titanium tetrachloride, which is then further purified and
! F  [! W9 Q# [  E. o- }converted to titanium dioxide by hydrolysis. The titanium dioxide is5 R# M( R# v6 }0 [) z2 A8 v
filtered, washed, and calcined./ }1 h# f8 l4 V% R$ d9 M. W) g
Commercial titanium dioxide may be coated with small amounts of
( \  k  a! ]6 Q4 j6 l+ Nalumina and/or silica to improve the technological properties of the2 F+ c0 F5 K; |5 d7 S
product.. o  U& Q8 p7 ]# k& y
C.A.S. number 13463-67-7
9 |: X! X7 ^9 v+ u5 I: o9 fChemical formula TiO2
& w# V4 [, y# I$ VFormula weight! S0 l# D; m- \+ T
79.88
. ]; _  T; n, H* k# bAssay0 I0 ^) r3 l" I+ z% t! s
Not less than 99.0% on the dried basis (on an aluminium oxide and
; X& ]5 [+ g" E# ]& S7 e( S5 qsilicon dioxide-free basis)
& v% G( p% z+ B4 DDESCRIPTION* K. e+ J% K: G  k3 m& f4 `( P
White to slightly coloured powder
( @* r! O# t( r0 X0 WFUNCTIONAL USES, e) c+ u7 q9 Z; v1 ]
Colour
- Z9 m$ M# a6 \+ Z4 `4 V9 K0 _CHARACTERISTICS6 |9 v6 e* @9 E9 Z' \
IDENTIFICATION
3 T" C- S% D5 S6 N3 M0 a  z$ f& |$ V, XSolubility (Vol. 4)
" y/ f& Y& l9 [6 }Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic2 t) k6 y2 m! f% S
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
% b  A8 Q+ H6 tsulfuric acid.5 h& r: A7 G5 K, @
Colour reaction6 k' F8 g' ~3 G( A
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
& E- v9 M$ L0 K- n3 B/ xsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with9 O6 P# ?' @5 T- N# v5 l+ A
water and filter. To 5 ml of this clear filtrate, add a few drops of4 M. p2 x7 i: E* q% X; e8 v9 \
hydrogen peroxide; an orange-red colour appears immediately.
* h' }3 z+ G7 b, J" P' d# h% v  \2 HPURITY2 J* B$ E& {1 x% S+ F
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)  O3 A+ J) r4 _; C
Loss on ignition (Vol. 4)
; t8 E/ Z7 E+ u! B! @4 {Not more than 1.0% (800o) on the dried basis( c& w7 o1 B4 a% ~
Aluminium oxide and/or% I  k, d2 r- T& n. P9 ?; v
silicon dioxide, U+ }- E+ e+ |7 n- n4 j' Q& U3 _. C
Not more than 2%, either singly or combined' k( o( H+ G( ]* ]. k# h
See descriptions under TESTS
& P) d4 ]( P- ]Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing( B5 K% Z1 K4 D# b2 v
alumina or silica.
9 t, ]- l# R  `$ nSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
$ F1 F  j$ z0 kplace on a steam bath for 30 min with occasional stirring. Filter
0 |6 q* _: U6 k% C- zthrough a Gooch crucible fitted with a glass fibre filter paper. Wash4 [, A0 t; }+ f/ W5 O  o
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
' l6 t# m& p0 P) ^  j2 L& Ocombined filtrate and washings to dryness, and ignite at a dull red
" B+ }! S/ e) R5 r. Sheat to constant weight.3 x; I5 c  a6 @
Water-soluble matter
# E. z9 E( M6 N$ G+ x/ ?' C(Vol. 4)7 ?9 `4 l4 P2 Y7 P5 I7 n, J! }
Not more than 0.5%
) H2 }/ ?5 X; WProceed as directed under acid-soluble substances (above), using. s% d9 v5 |4 x3 ]& m
water in place of 0.5 N hydrochloric acid.! m/ ?# |" r7 x5 r) T; Q! n  U
Impurities soluble in 0.5 N/ d3 d" Q, L' @2 U: `
hydrochloric acid
/ @: \8 U5 a6 e9 X% y- y: FAntimony Not more than 2 mg/kg
* ]  n: r) |9 B; b; R9 R5 ESee description under TESTS
9 o  h0 h2 q( n" C% l' T( PArsenic Not more than 1 mg/kg( R) J+ C+ x" `) Q1 R
See description under TESTS7 ]6 W+ ~$ o3 |5 {
Cadmium Not more than 1 mg/kg! D& |! G6 ?- s5 r8 t5 e
See description under TESTS
; l: E! I( K( l1 ?Lead% i# m; K3 P2 f' `1 _
Not more than 10 mg/kg
2 N9 W8 R# y) Y$ z1 _- ySee description under TESTS  C4 x+ ]/ a( B$ X6 c; V
Mercury (Vol. 4) Not more than 1 mg/kg
( n/ |& L) S% a" g. tDetermine using the cold vapour atomic absorption technique. Select a6 h; j- R" A' G4 ?# ^
sample size appropriate to the specified level6 |  o6 M4 b  b- h
TESTS: a* U; A& Q) J$ j8 E
PURITY TESTS2 h0 {9 Y: r: b2 x3 S8 N- v
Impurities soluble in 0.5 N7 a5 T1 Z- u/ @" G
hydrochloric acid
! i7 S7 ^8 M- z! y( |6 o* ^Antimony, arsenic,
+ I1 t& ~1 H* x1 r8 U; lcadmium and lead; S  x) N' _6 J/ U8 G
(Vol.4)
: _; t9 R1 v) \) Y) ]Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N$ g9 s' e9 z, s4 ]$ U
hydrochloric acid, cover with a watch glass, and heat to boiling on a
: C% X; w0 h9 Rhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
0 j4 K) f5 g" \# Bcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved" Z4 f4 X8 j, k9 u& J$ J0 o. E
material settles. Decant the supernatant extract through a Whatman
! B+ a% h& K0 cNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
; h5 A! s9 A4 Z( i' H. Kvolumetric flask and retaining as much as possible of the undissolved
! S) l) d; {7 f$ k& y6 jmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
. O3 J) e0 P( P  V6 W1 x' y/ [) Q& m% |beaker, washing off the watch glass with the water, and pour the4 p% ~& [/ J" r' U+ C# k# D9 M* [0 L/ W
contents into the centrifuge bottle. Form a slurry, using a glass stirring
& B! @9 l( B  R8 {, frod, and centrifuge. Decant through the same filter paper, and collect5 ]9 {0 |1 @9 U
the washings in the volumetric flask containing the initial extract.
# f. J4 o( z) l, f9 ~! x- ZRepeat the entire washing process two more times. Finally, wash the3 s5 a; w$ b+ k8 h0 y) {5 V
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask( z" c' a# b- t: i* U
to room temperature, dilute to volume with water, and mix.
( @7 N# ~# M' cDetermine antimony, cadmium, and lead using an AAS/ICP-AES
1 a0 N! p% f9 F3 I8 `  ntechnique appropriate to the specified level. Determine arsenic using the6 X4 X1 W: B9 q& x1 r+ S% x# K
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using/ t: E% n  V4 P4 C1 d/ s
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
! {0 t2 C% D# @( q; C1 g. The selection of sample size and method of sample preparation
, o9 R0 D: K; }9 q9 x0 Bmay be based on the principles of the methods described in Volume 4.
& W) D. f% b+ m, w; @& s# K, qAluminium oxide Reagents and sample solutions  r8 k: Z' k# O% N
0.01 N Zinc Sulfate( {5 \+ m$ Y6 A) j0 N
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
  N; L1 p- @4 Lmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg, W2 l1 ^5 D$ b: q/ Y
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of+ u0 v( y1 y: {$ W
concentrated hydrochloric acid, heating gently to effect solution, then! y2 P6 s; {  F  e) c. P
transfer the solution into a 1000-ml volumetric flask, dilute to volume# K1 F( T8 h5 h5 b8 \. h5 u
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500! l1 V' w" z1 C1 N" M0 J
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
" B) Z  e2 w( d$ x. ]! x$ t5 `9 c3 Rconcentrated hydrochloric acid, add 1 drop of methyl orange TS and4 `4 r( N" b5 g( g
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,% a/ X3 l# @4 X+ P
dropwise, ammonia solution (1 in 5) until the colour is just completely
+ i- q- n- r0 @changed from red to orange-yellow. Then, add:
# U# G# q& O4 E" }$ S9 |! A) S(a): 10 ml of ammonium acetate buffer solution (77 g of% N9 H! e# ^8 J" r' O8 Y
ammonium acetate plus 10 ml of glacial acetic acid, dilute to3 h$ E4 p2 D$ b  B
1000 ml with water) and1 `: I; l* U8 b4 b% {7 A
(b): 10 ml of diammonium hydrogen phosphate solution (150 g" T: o, [& c9 S: e1 `' _
of diammonium hydrogen phosphate in 700 ml of water,
3 h3 g* Q* i2 D: A* cadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
$ s2 u. d$ w* h1 i1 l' {then dilute to 1000 ml with water).7 @+ Z' m. d% h3 @; x  j
Boil the solution for 5 min, cool it quickly to room temperature in a
) ?: v0 [0 [; t: |; tstream of running water, add 3 drops of xylenol orange TS, and mix.
5 s4 ~- b7 b0 @: J* G/ i8 KUsing the zinc sulfate solution as titrant, titrate the solution to the first
. e: [* x5 ]. q9 @; L, lyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:+ ]9 W& t+ u+ y7 N
This titration should be performed quickly near the end-point by# a% R4 X& Y1 O; w; b5 ^- B
adding rapidly 0.2 ml increments of the titrant until the first colour2 r; U) S- F7 i1 l
change occurs; although the colour will fade in 5-10 sec, it is the true6 ]) r0 x5 O1 q9 T9 c3 X% N
end-point. Failure to observe the first colour change will result in an
- z( [6 Z  t$ o4 r  g( A) K9 E3 sincorrect titration. The fading end-point does not occur at the second3 \2 s# \$ E  q# y1 Y# k0 I
end-point.)
- D3 _' \5 d' V% l! _8 B6 WAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a( t( [+ T8 I$ @2 E( e
stream of running water. Titrate this solution, using the zinc sulfate
- s2 e  A7 Z4 }solution as titrant, to the same fugitive yellow-brown or pink end-point
8 ]* Z4 E9 x; D- U# c% Das described above.% w# p4 n* l6 W" X- d7 n5 `
Calculate the titre T of zinc sulfate solution by the formula:
: }0 S& h& b- J3 z4 V7 O* ET = 18.896 W / V; w+ b( o- s6 q! E& l
where7 U6 j0 s; j! R9 k
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
5 }+ P  x- E+ N- A' P5 hW is the mass (g) of aluminium wire
( }1 E! a" k$ o* q9 e  hV is the ml of the zinc sulfate solution consumed in the! v& i* v& l3 D/ ~) T8 y4 P
second titration
, f; ?! z* u: [$ E18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
7 Y2 w5 y* k/ A% qR is the ratio of the formula weight of aluminium oxide to
. U7 M7 F" I* c  _2 X/ `' wthat of elemental aluminium.
% b, p- g1 n7 t9 _' X7 L- `Sample Solution A7 f) R5 [. R! u8 W( R  @
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica/ C' V6 a3 l  a0 e7 h
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).* ?6 @6 W" n$ s! _" X4 n
(Note: Do not use more sodium bisulfate than specified, as an excess
% @: k; i. ?' d" E( _8 @/ {concentration of salt will interfere with the EDTA titration later on in the
1 `- ?1 ^2 u  @$ sprocedure.) Begin heating the flask at low heat on a hot plate, and
* ^  {# N- p$ Sthen gradually raise the temperature until full heat is reached.
9 {+ x2 j+ G7 P/ |- H(Caution: perform this procedure in a well ventilated area. ) When6 P. N0 n) E! m  J
spattering has stopped and light fumes of SO3 appear, heat in the full
+ x( V: d+ Y. I5 g; \flame of a Meeker burner, with the flask tilted so that the fusion of the
& k4 p7 @, L# a- C* V% B' i) I8 Q9 r9 ?sample and sodium bisulfate is concentrated at one end of the flask.
  z2 v: }" Z6 m9 n/ g% E" T- g, nSwirl constantly until the melt is clear (except for silica content), but
& b1 T8 Z; W. mguard against prolonged heating to avoid precipitation of titanium
: T$ W/ c! p: _7 odioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
5 M, ?2 \; F2 K' }2 othe mass has dissolved and a clear solution results. Cool, and dilute to
# f/ g" }) z/ U" y+ m120 ml with water. Introduce a magnetic stir bar into the flask.
9 V( ~, X8 f; {' r, K) l& [Sample Solution B
, T3 Y% b3 v; f4 C2 sPrepare 200 ml of an approximately 6.25 M solution of sodium! B5 J2 y0 Y6 I& g* }+ \8 i: h. C
hydroxide. Add 65 ml of this solution to Sample Solution A, while
# k( T2 p" d* Fstirring with the magnetic stirrer; pour the remaining 135 ml of the
- K$ u; R2 w4 u" j& walkali solution into a 500-ml volumetric flask.
3 E1 p: \, }( _& X8 H$ V' b$ w0 L  rSlowly, with constant stirring, add the sample mixture to the alkali
8 B8 r% o4 P; I) ^2 Jsolution in the 500-ml volumetric flask; dilute to volume with water,
7 w8 f3 e+ z! s: Q0 }/ E8 R. wand mix. (Note: If the procedure is delayed at this point for more than, }' G  W& j4 N9 K! Z* T$ Y
2 hours, store the contents of the volumetric flask in a polyethylene' Z7 ~7 w, \$ ?5 c6 \
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),) }# z% `$ U& r
then filter the supernatant liquid through a very fine filter paper. Label" Y  h" w, Y, N9 `
the filtrate Sample Solution B.' c8 A8 d/ K4 C, y+ Q
Sample Solution C+ |$ W- i7 g& ~& D3 o6 Y
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
% k) m1 x. n8 G% \7 U* ~. V. @flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid" Q  j; t) }1 z
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02: D6 W/ ~& {$ `0 o, ], G
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
! B" ^3 S2 V3 z) Q: G1 S; t' `0 Rknown, calculate the optimum volume of EDTA solution to be added
0 B8 B5 I8 F  j9 X$ u  u$ Jby the formula: (4 x % Al2O3) + 5.]
1 B4 P" k5 x: OAdd, dropwise, ammonia solution (1 in 5) until the colour is just& e: l2 }4 B. t. Y. V
completely changed from red to orange-yellow. Then add10 ml each9 a- ~" z* w6 @# ~' y0 ?$ {
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to1 W3 m# e8 m' K" A8 O! {
room temperature in a stream of running water, add 3 drops of xylenol/ z. B1 A- R. y& a
orange TS, and mix. If the solution is purple, yellow-brown, or pink,: F+ o' ?: c! a! o: N4 p
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
& l5 [" w( d+ p, z' j2 ipH, a pink colour indicates that not enough of the EDTA solution has
& j4 ~$ ]5 \! v  ~0 I+ {been added, in which case, discard the solution and repeat this1 Y  M6 U& L  S# @' U, V. r+ V
procedure with another 100 ml of Sample Solution B, using 50 ml,
/ W, W1 h! }8 H' vrather than 25 ml, of 0.02 M disodium EDTA." A8 B) `5 b& p, o) b9 k
Procedure
2 }# e- g5 s# M( q' nUsing the standardized zinc sulfate solution as titrant, titrate Sample3 f/ C/ R9 m1 `/ \* I/ u* L
Solution C to the first yellow-brown or pink end-point that persists for
2 i# C8 ~; A. A; @" `5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
0 A+ S5 G$ N5 F% F6 q) e* @titration should require more than 8 ml of titrant, but for more accurate) m# k6 ^8 h6 G7 x
work a titration of 10-15 ml is desirable.
' Y6 k+ h3 H8 CAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
9 }) t4 b# z/ Z* Imin, and cool in a stream of running water. Titrate this solution, using
; P( h6 y* h$ O1 @! Bthe standardized zinc sulfate solution as titrant, to the same fugitive
& l' n; v0 i) k) J" h5 Q1 k# Uyellow-brown or pink end-point as described above.' i4 M2 u" x3 u% u  E' M
Calculation:
0 c7 K# h4 m, t3 o+ _# y; ]Calculate the percentage of aluminium oxide (Al2O3) in the sample
. B1 L5 O% S4 x6 ]taken by the formula:
5 |* {/ O$ M3 h$ ]! ?: p. X% Al2O3 = 100 × (0.005VT)/S
4 t0 v. j) @" x: \where
& g( z$ ?9 u6 i. h! eV is the number of ml of 0.01 N zinc sulfate consumed in
( I+ b7 ~% x, g: O* jthe second titration,4 R; g$ n6 m) h7 p! i
T is the titre of the zinc sulfate solution,
: `) M: S, o% B0 @$ NS is the mass (g) of the sample taken, and
$ k5 ]# P  u( |3 j3 p3 b7 a3 z0.005 = 500 ml / (1000mg/g × 100 ml).4 }5 ~  I+ s% ]' o
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
$ a; r) Z9 h+ P: Cglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).) ^! Z1 Z; M& u- k7 A& y/ V* A
Heat gently over a Meeker burner, while swirling the flask, until
& b. f; ?# w) C  Mdecomposition and fusion are complete and the melt is clear, except3 ?% ^8 ?6 N. i, ?0 \
for the silica content, and then cool. (Caution: Do not overheat the: E- W- N  V6 v# x0 o
contents of the flask at the beginning, and heat cautiously during( O8 `9 t/ _, p
fusion to avoid spattering.)
& M3 ?9 I9 @- T; W( D6 p" c( L% H9 aTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
- X' q" I1 k! _# m9 n, t' V8 dcarefully and slowly until the melt is dissolved. Cool, and carefully add# t9 L, Q. V5 y6 A" O3 e! B
150 ml of water by pouring very small portions down the sides of the7 `7 s* p, O, D6 H+ U
flask, with frequent swirling to avoid over-heating and spattering. Allow
( T2 }( I) ^) pthe contents of the flask to cool, and filter through fine ashless filter
0 }1 O, D/ G/ V; u; x5 a3 Kpaper, using a 60 degree gravity funnel. Rinse out all the silica from
- `( {% p9 W& l( j1 M0 y4 Uthe flask onto the filter paper with sulfuric acid solution (1 in 10).
% E6 E/ P1 C5 Y' Z' {Transfer the filter paper and its contents into a platinum crucible, dry in
5 b9 _5 m3 t& L' \4 [; h5 qan oven at 1200, and heat the partly covered crucible over a Bunsen; \8 s* l2 f7 W
burner. To prevent flaming of the filter paper, first heat the cover from
' H. ~! T! E. [: labove, and then the crucible from below.
$ g: {" d7 G0 }; T( yWhen the filter paper is consumed, transfer the crucible to a muffle
5 t3 B9 N: R7 V% s! I4 U. j, B' B! Dfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
1 D* Y2 r& |1 S: t/ o2 pweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated. `9 A0 a3 Y1 J4 U# ~( k% |: Y* |
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first$ Y. \  j2 Z" M' O9 B
on a low-heat hot plate (to remove the HF) and then over a Bunsen  @5 a! [$ T8 K3 f3 I7 a0 X
burner (to remove the H2SO4). Take precautions to avoid spattering,1 u* w! R' E. [2 [, x) m
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a5 N) D0 p0 Z2 d
desiccator, and weigh again. Record the difference between the two4 R  p& `: X3 V2 V% s' ?( n
weights as the content of SiO2 in the sample.
6 s# K' B; b& c4 d& C/ y0 l- VMETHOD OF ASSAY  g% S! _, h8 l
Accurately weigh about 150 mg of the sample, previously dried at 105o0 z' S7 L' t" i% G+ e
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water) y! k$ W, r. d( J8 ?
and shake until a homogeneous, milky suspension is obtained. Add 309 V6 x$ s# K- l* L: A4 e, T/ g$ A
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
8 G: M! r2 y2 m: }! b& Zheat gently, then heat strongly until a clear solution is obtained. Cool,
4 ]) d* A9 F- K1 Wthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
! A2 w9 v  |* h- Y7 k: Kacid, and stir. Add 3 g of aluminium metal, and immediately insert a2 p: E# O8 y. @3 j5 o4 l1 K5 ~
rubber stopper fitted with a U-shaped glass tube while immersing the
- V. a* Z, a3 y8 A: _7 k: Lother end of the U-tube into a saturated solution of sodium6 |$ c! N6 f( t/ e3 X4 D) v/ v
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
3 x/ a) W& s. y1 F8 q3 J* Zhydrogen. Allow to stand for a few minutes after the aluminium metal$ {7 i" Y; x5 E- F. h. S# q0 u
has dissolved completely to produce a transparent purple solution.
7 A* n6 \" l( ?4 b0 r7 I0 t7 TCool to below 50o in running water, and remove the rubber stopper
# S( }; Z4 u% M3 k: ucarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate' j1 L) n# m) f6 D
solution as an indicator, and immediately titrate with 0.2 N ferric
2 ^; j# `' ~. q3 I9 N( `+ tammonium sulfate until a faint brown colour that persists for 30
- E9 G! a' |* F; Mseconds is obtained. Perform a blank determination and make any: z  ]4 q" P6 o" I: Z& Q
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
% {1 J! h+ u% {$ F! Qequivalent to 7.990 mg of TiO2.
+ ?4 t1 e; T" f$ p' ]
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