标题: 二氧化钛(钛白粉) [打印本页] 作者: 1123456789 时间: 2008-5-23 12:09 标题: 二氧化钛(钛白粉) 二氧化钛(钛白粉) $ k* ^( E4 b- i. `0 T+ ? : _- V9 D& G3 f; n8 m- O7 ?' |6 K
CAC关于二氧化钛(钛白粉)的使用规定# q# n, e t+ ~* J b: ^' t8 m
GSFA Online 7 r$ T2 n7 \) NFood Additive Details 3 s5 @2 l! @/ M" fTitanium Dioxide (171) 4 q& E0 J% N2 z( s) @: ^. ONumber Food Category 8 h/ H5 f {' L7 k( b
01.1.2 Dairy-based drinks, flavoured and/or fermented (e.g., chocolate milk, cocoa, eggnog, drinking yoghurt, whey-based drinks) g: o5 @3 D5 }) V 01.3 Condensed milk and analogues (plain) & ], O& ^ I2 N# d2 z 01.4.3 Clotted cream (plain) 5 y5 c# T1 r+ l5 E6 w 01.4.4 Cream analogues 5 H# V7 D2 Z" x 01.5 Milk powder and cream powder and powder analogues (plain) % B3 v. ~' p$ d) u4 ~! `
01.6 Cheese and analogues . o' i; g5 ?5 A# i$ W
01.7 Dairy-based desserts (e.g., pudding, fruit or flavoured yoghurt) : u! h$ ^% x% V% f/ j( F
01.8 Whey and whey products, excluding whey cheeses $ S3 d9 b# Z+ s- K# C, v
02.2.1.2 Margarine and similar products 4 L- _: p3 D4 @- U2 W7 N5 R3 ~ 02.2.1.3 Blends of butter and margarine & f9 w i2 g9 a2 H 02.2.2 Emulsions containing less than 80% fat z# y6 v, Z2 Q4 F9 K1 q @ 02.3 Fat emulsions maily of type oil-in-water, including mixed and/or flavoured products based on fat emulsions 9 F0 m9 l0 y; ^) f0 Q 02.4 Fat-based desserts excluding dairy-based dessert products of food category 01.7 ; D; y y# D* ?6 \0 ? 03.0 Edible ices, including sherbet and sorbet 5 }/ U) o0 |1 ]
04.1.2 Processed fruit 9 {2 j+ R, |! E/ A( y 04.2.2.2 Dried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweeds, and nuts and seeds ' D+ {- R. E' w8 t
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 j! E% ]; p C# B. f8 L
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 & W9 Y* {3 p$ O% _9 G2 D 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) U/ g8 _" B: B, b- M 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 1 ]9 L {( T; g9 p, d) j5 G$ i0 r w
04.2.2.8 Cooked or fried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds & ]) _3 @5 H% U3 _( w- d: _( k
05.0 Confectionery & [: f: `3 [1 x0 Q0 S9 e7 q& h7 w
06.3 Breakfast cereals, including rolled oats $ p; R3 i7 q1 }" R 06.4.3 Pre-cooked pastas and noodles and like products " V+ Q6 ?$ A/ F 06.5 Cereal and starch based desserts (e.g., rice pudding, tapioca pudding) ; m, r8 E+ F3 Y' Q8 V7 Z: L8 e
06.6 Batters (e.g., for breading or batters for fish or poultry) / L6 S# U2 v4 N8 P d! }4 c
06.7 Pre-cooked or processed rice products, including rice cakes (Oriental type only) + Y1 |$ h/ G( h9 ] 06.8 Soybean products (excluding soybean products of food category 12.9 and fermented soybean products of food category 12.10) 4 Z% E5 V. @& l p: K 07.0 Bakery wares 6 E0 G A7 X K4 z% w# {
08.2 Processed meat, poultry, and game products in whole pieces or cuts % Y% h* Y8 n! \/ X# [5 L
08.3 Processed comminuted meat, poultry, and game products ) y, d# B) O6 b
08.4 Edible casings (e.g., sausage casings) ' k! m9 Y) F2 _2 q. L+ F 09.3 Semi-preserved fish and fish products, including mollusks, crustaceans, and echinoderms 3 C/ F1 R. C, u0 v; j1 _7 r# a7 x
09.4 Fully preserved, including canned or fermented fish and fish products, including mollusks, crustaceans, and echinoderms 5 @3 A8 Z. e. {. D 10.2.3 Dried and/or heat coagulated egg products % F. _8 ~9 ~/ Z 10.3 Preserved eggs, including alkaline, salted, and canned eggs 2 X& t8 b% |5 H9 G+ D) ~* K* C 10.4 Egg-based desserts (e.g., custard) 6 f2 N0 f) G: l0 P2 }& c
11.6 Table-top sweeteners, including those containing high-intensity sweeteners 8 G0 W/ L5 _' B S: v) U 12.2.2 Seasonings and condiments $ e4 e( w" @2 c
12.3 Vinegars 2 {1 M. {7 [" x/ Y* w+ `+ ^" E: O
12.4 Mustards * A- ?4 i- B* N. J( c 12.5 Soups and broths ( `. [1 z' r( `3 k8 g. K5 N6 G( h, k
12.6 Sauces and like products 5 i0 {% a/ O7 Y# Q. D$ d' N 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 9 x8 |, g' j9 Q3 y/ t8 C1 e) D 12.8 Yeast and like products n" d6 F$ C( Y, A
12.9 Protein products + B, z: J* q% }& S, f 12.10 Fermented soybean products 1 q4 u- }2 w) O# K+ E$ |+ f 13.3 Dietetic foods intended for special medical purposes (excluding products of food category 13.1) 0 l5 f, m' u& Q- f0 b/ a$ C 13.4 Dietetic formulae for slimming purposes and weight reduction 8 U( ?# C" ~$ \
13.5 Dietetic foods (e.g., supplementary foods for dietary use) excluding products of food categories 13.1 - 13.4 and 13.6 " \0 f+ R% [) y$ Y! a# ?
13.6 Food supplements : t5 ^6 d# ~7 j: r5 I8 g
14.1.1.2 Table waters and soda waters 1 v4 G% T4 _! O2 P) J
14.1.4 Water-based flavoured drinks, including "sport," "energy," or "electrolyte" drinks and particulated drinks # A8 T, \( O. l
14.2.1 Beer and malt beverages ( C( z" M7 W: F
14.2.2 Cider and perry 8 Z! H& K* Z3 p
14.2.4 Wines (other than grape) # f( `4 ~ ?% r7 f* t1 z5 {; M7 }; G 14.2.5 Mead : _% J3 i% e* Y6 e& p5 k9 q! D
14.2.6 Distilled spirituous beverages containing more than 15% alcohol $ ]+ l7 V7 }- G
14.2.7 Aromatized alcoholic beverages (e.g., beer, wine and spirituous cooler-type beverages, low alcoholic refreshers) 4 ~3 V, g' D. D. K8 G
15.0 Ready-to-eat savouries 3 [/ e2 u. d/ i8 U( D3 b0 z5 W
16.0 Composite foods - foods that could not be placed in categories 01 – 15 ^! w+ K: p: K: @# I; c; G; N3 H) \- }0 i6 h" y: W# a
6 A8 o# x! P J
部分译文:3 ?" s# W: Y' g/ T5 P% n6 q7 k' J
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食品添加剂通用规则 1 H; o. A3 T' X% i3 q' G5 P" M食品添加剂 3 r6 d% r1 U. J; C, k$ A8 T 二氧化钛(171) " Q3 D, p! o x5 C, e e食品类别: $ F5 A+ N4 _, k3 X. v06.3 早餐谷类,包括燕麦片 5 U$ i: S1 @, o! U( {4 g' S3 Y06.4.3面条及类似产品 + l) W- _; I) l3 q4 C: d+ S06.5 谷类,淀粉甜点(包括:米粉布丁,木薯布丁) 2 O# B# J2 L( h# X06.6 面团 , g6 d+ v- B3 m7 Y* e' l$ z9 ]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 # G0 W* L$ g) _( S- s
07.0 烘焙类) K7 u; W* ]$ H
07.1 面包,普通烘焙类,以及其混合物3 h2 L3 [3 a. V- T5 f Y
07.1.1 面包,面包卷3 l. S# t( Z# f( m, [8 ^
07.1.1.1 酵母发酵面包及特殊面包' k8 \% q6 z3 L* a0 o) C. O
07.1.1.2 苏打面包 - e% ]! j/ o" ]; |1 {7 O, a0 G5 z# R1 g( s7 b" k7 @, P! G
1 m# ]( `6 y$ K$ j4 s 作者: 1123456789 时间: 2008-5-23 12:10 标题: 二氧化钛(钛白粉) 二氧化钛(钛白粉) 0 ~& U" e1 C4 l# [ ( N2 [9 G' k( u4 ]' M: Z* mJECFA关于二氧化钛(钛白粉)的结论; X% ?6 u1 I* B# n, y% X
+ b0 f# F j1 N5 N8 a
摘要: 2006年JECFA关于二氧化钛的结论4 f" b' y! b9 S. R4 M
ADI值:不作限制。& l% w! E* V. b" ?
功能:着色剂7 v; V+ v; Q% ^0 P6 q# w; Z8 J
& z+ M/ _4 \, r+ G2 N/ ?TITANIUM DIOXIDE & w# B, \7 _) @$ JPrepared at the 67th JECFA (2006) and published in FAO JECFA* F* G; T9 D. y# Z {3 z) x5 R
Monographs 3 (2006), superseding specifications prepared at the 63rd' h( W6 T, R0 C! f
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the( s$ J9 h2 z2 B$ i# Z% Y* Y
Combined Compendium of Food Additive Specifications, FAO JECFA / a6 s" m3 w b# k. p# ~Monographs 1 (2005). An ADI “not limited” was established at the 13th & I X* o! O* g4 NJECFA (1969). : H6 b9 U9 q4 ?/ TSYNONYMS# p7 v* M+ X0 Y! i" K+ X$ R
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171+ p+ {2 G6 T4 }: E9 m# r2 `7 A
DEFINITION8 v3 r' k4 G! a; r" Y
Titanium dioxide is produced by either the sulfate or the chloride ' }4 {* E* c9 c. x# Aprocess. Processing conditions determine the form (anatase or rutile8 L2 [1 s2 d+ h; P2 Y2 Y
structure) of the final product. c i" q7 @+ A/ PIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)' z; h, ^ B* t% _! I
or ilmenite and titanium slag. After a series of purification steps, the4 ^1 z6 R9 N3 ]6 I# K |! G& v
isolated titanium dioxide is finally washed with water, calcined, and 0 M! f& {" [# }7 k; G, X, d( @micronized.1 x( }8 N7 B; |
In the chloride process, chlorine gas is reacted with a titaniumcontaining . m0 I1 `' {* f. J7 J G+ t3 emineral under reducing conditions to form anhydrous$ L1 c% I0 }; x4 R% V
titanium tetrachloride, which is subsequently purified and converted to ' }9 M( \6 W$ s( Vtitanium dioxide either by direct thermal oxidation or by reaction with 4 h, T8 }& e, hsteam in the vapour phase. Alternatively, concentrated hydrochloric 0 M9 B: d, t7 Z7 ^$ Dacid can be reacted with the titanium-containing mineral to form a ; s! @% u+ D$ Y. s4 I- h: z0 c6 ysolution of titanium tetrachloride, which is then further purified and 3 ^2 E! b5 ?9 ~* Bconverted to titanium dioxide by hydrolysis. The titanium dioxide is 2 t! M5 `* `% x3 ]. bfiltered, washed, and calcined.. e! f) q# B8 B4 l9 K
Commercial titanium dioxide may be coated with small amounts of : {: `- z+ m) c5 w' H5 O7 ]alumina and/or silica to improve the technological properties of the& q. Y5 f- `$ G+ R% g8 [; Z
product.# K) T; g5 F- d. C0 j
C.A.S. number 13463-67-7 0 W" F7 Y- r$ \$ B; Q* ]2 OChemical formula TiO2; h& q- g5 J# l. q' }& i4 r
Formula weight ( d. R# F# L+ K9 s1 J _79.88 # B0 ?! Q1 G4 x0 k4 PAssay 1 X1 r( V/ E9 RNot less than 99.0% on the dried basis (on an aluminium oxide and 2 v/ }/ M& o6 `1 |silicon dioxide-free basis)+ J1 `; R" d6 {' ~4 l. w4 d
DESCRIPTION* `- [; B0 L I: d
White to slightly coloured powder ; B( O! [* C" Z* ^% E5 DFUNCTIONAL USES 7 P; o2 t! j8 l: y8 N* L Z( eColour ' O; p& v" K+ y# A6 k6 J# xCHARACTERISTICS # s) q( f! U/ hIDENTIFICATION 7 ~/ z. j! w( B- c# T; e! eSolubility (Vol. 4) . s% ~' [+ m/ P( G. j# ?Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic 9 l4 \: Y* m! L. |; u! S, E: usolvents. Dissolves slowly in hydrofluoric acid and hot concentrated0 Q/ Y7 }* d9 v+ v( X
sulfuric acid. 5 l7 B- i, O8 ^4 CColour reaction4 m" J: K5 O+ n$ h
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of, q! I8 y: W4 J+ N/ \' u
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with . @. @: a* z2 q, Jwater and filter. To 5 ml of this clear filtrate, add a few drops of 1 p; Z) g4 o G5 hhydrogen peroxide; an orange-red colour appears immediately. ) p, `+ ]! a" wPURITY ) t6 q4 Q* \4 g7 w; a" H {/ w3 fLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h) 3 W* Q& z, h: G3 R( X- nLoss on ignition (Vol. 4)" H: o& [4 `2 R7 H( b
Not more than 1.0% (800o) on the dried basis! Q8 s5 @. Y) T. U2 v% A' P
Aluminium oxide and/or 4 D& Q% R, N( C: Hsilicon dioxide + a. g1 n" {( p+ `4 d! `! }. G" oNot more than 2%, either singly or combined 8 ?7 j z7 _9 u$ l8 gSee descriptions under TESTS 3 A. x S3 s, XAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing * i7 K5 e+ ?, I) U. Z% ^alumina or silica." V3 T& J# I4 R* N% D1 L
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and* |) U7 h- _) A
place on a steam bath for 30 min with occasional stirring. Filter : x! P% b/ I3 |# J& U: Fthrough a Gooch crucible fitted with a glass fibre filter paper. Wash , s7 n; u) l! N0 m; ]with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the 8 X) V! }; |* [0 m P P2 ^combined filtrate and washings to dryness, and ignite at a dull red- b+ h) _1 h7 ^; Y3 w, a
heat to constant weight.0 G8 l* I9 n3 p
Water-soluble matter; T' v' b ?7 w# s5 P5 G9 P9 I+ z
(Vol. 4)4 D B( i3 q6 z+ [. R9 O% f' S
Not more than 0.5% 9 J8 s* p: M- @$ h. B _$ zProceed as directed under acid-soluble substances (above), using ) V# v ^: f) S/ f# y9 `* m3 Lwater in place of 0.5 N hydrochloric acid.; _/ s0 s; c h6 n$ p) Y
Impurities soluble in 0.5 N ! l% ~" g9 Z: u9 ehydrochloric acid: d8 S9 O. n4 V; P8 }. F7 @, s+ y; S2 `
Antimony Not more than 2 mg/kg' d( n# S' r+ o5 z' ~" e
See description under TESTS & R: F- A/ @( x1 a D8 w' LArsenic Not more than 1 mg/kg 0 i* r4 c9 g% G' L! b3 Q! VSee description under TESTS# p/ [' ?* I- G; E M0 T
Cadmium Not more than 1 mg/kg& w( l% |; k; z$ {
See description under TESTS$ W$ [+ B8 c- B$ _* |* s* p( c6 x" w
Lead* k3 d z, f; U3 B# |
Not more than 10 mg/kg # H( }1 I% o& {. ~( e2 ^3 ISee description under TESTS7 a$ s# l- s- C7 V6 R0 v& C$ l
Mercury (Vol. 4) Not more than 1 mg/kg ) e) A, x; ~0 k8 x* n6 m' pDetermine using the cold vapour atomic absorption technique. Select a : g6 d7 G4 O0 k% Y5 v/ Ssample size appropriate to the specified level - V: K( r$ t. J' jTESTS. l2 a6 s; M9 X K
PURITY TESTS0 A5 l Q- d/ O# u+ |1 H+ o
Impurities soluble in 0.5 N - e* q& h$ R X" o7 H. k+ O5 N# \hydrochloric acid# L* ~& Y/ X9 r/ \
Antimony, arsenic,1 N4 X7 T- q6 @% ~3 w
cadmium and lead% e# F: I: H/ w1 [. n9 b
(Vol.4)0 t# E* k3 |' ?+ X& l
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N & \1 {2 P) \& b' f! w* E3 E( R% U+ S8 @! Ghydrochloric acid, cover with a watch glass, and heat to boiling on a , L) i7 y9 Y! Mhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml1 y% ]9 j0 U! s7 q
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved 3 N6 R; U( `" C' r* zmaterial settles. Decant the supernatant extract through a Whatman ; r+ y9 ] @: ^/ PNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml 9 |" Z. F5 }2 U$ v' Q" k4 ovolumetric flask and retaining as much as possible of the undissolved 9 D. `% |! D# ^& Ematerial in the centrifuge bottle. Add 10 ml of hot water to the original, F( S, v. @- F$ A' |2 t( E
beaker, washing off the watch glass with the water, and pour the8 R. W9 d, I5 e& m( q. C
contents into the centrifuge bottle. Form a slurry, using a glass stirring 8 }0 x' R4 }% G, grod, and centrifuge. Decant through the same filter paper, and collect0 m, L" ^! F* W2 E8 O
the washings in the volumetric flask containing the initial extract.$ l5 ?% f2 C! B, o
Repeat the entire washing process two more times. Finally, wash the* S& h5 c) |& @2 F. ^
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask) Z- d4 Z. P2 s" Q7 I, \7 V
to room temperature, dilute to volume with water, and mix. ; E+ ^$ `7 ]* m/ VDetermine antimony, cadmium, and lead using an AAS/ICP-AES 3 X3 V# T4 j5 \$ W5 a. wtechnique appropriate to the specified level. Determine arsenic using the0 F: X* P$ e$ L5 |' G5 M- w k R
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using! u% e4 U; _3 z* j* K/ D% F
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than. a3 m- w) ^1 t$ r* o: H" S2 ]
1 g. The selection of sample size and method of sample preparation - a/ Z0 W+ |' [! c( F4 `7 b1 {may be based on the principles of the methods described in Volume 4.) j/ F. y# Z1 d+ t9 I/ G8 C
Aluminium oxide Reagents and sample solutions / U7 ]! Z" o# ]$ r5 ?) B; {9 }0.01 N Zinc Sulfate+ w0 l# q( y: P8 _/ Q
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to- G: C4 ?" T3 ^( v9 @8 D
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg8 x8 @# B6 y: b
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of9 z2 D5 z$ R9 i2 l: W* V
concentrated hydrochloric acid, heating gently to effect solution, then & [, T$ q- g$ Q7 Y! @transfer the solution into a 1000-ml volumetric flask, dilute to volume. }( f% r/ e2 p6 r' l
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500 % F/ ?0 W* g5 d0 ?ml Erlenmeyer flask containing 90 ml of water and 3 ml of $ C2 b9 d x1 C4 W% j- {concentrated hydrochloric acid, add 1 drop of methyl orange TS and) j" N; b6 T. a1 X# O; q
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add, . i3 r1 t2 c9 X/ E7 `. \- Q* }% `dropwise, ammonia solution (1 in 5) until the colour is just completely# b: `: c: B$ B6 h( T+ l
changed from red to orange-yellow. Then, add:" k9 m8 t/ T" j7 }: g
(a): 10 ml of ammonium acetate buffer solution (77 g of 5 q5 w8 @! b! K- k# S! dammonium acetate plus 10 ml of glacial acetic acid, dilute to6 o, n9 ]# f/ f6 f; i6 z5 e& i" w
1000 ml with water) and$ P- X8 Y! o5 x( L1 O
(b): 10 ml of diammonium hydrogen phosphate solution (150 g, ?$ ]6 ] E. m- N5 j
of diammonium hydrogen phosphate in 700 ml of water,. E+ Q9 a" v5 A; E h- ^- {0 N
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,3 z/ @# P6 x+ h0 b
then dilute to 1000 ml with water).. z d, C. ?6 `9 ~( a% R
Boil the solution for 5 min, cool it quickly to room temperature in a# N8 |6 M' a ~- U Y) O
stream of running water, add 3 drops of xylenol orange TS, and mix. , W: l. m2 e3 \Using the zinc sulfate solution as titrant, titrate the solution to the first . ~! t7 {3 C2 X( C0 i) c) ~yellow-brown or pink end-point colour that persists for 5-10 sec. (Note: ; `8 s% r& W3 Q4 W8 N+ z* eThis titration should be performed quickly near the end-point by 3 ]+ O& M$ E. d# [, d( U" G: b5 Eadding rapidly 0.2 ml increments of the titrant until the first colour0 a+ J9 l9 Y2 U5 p* o$ M
change occurs; although the colour will fade in 5-10 sec, it is the true 1 F4 v9 p0 \6 ~, { h eend-point. Failure to observe the first colour change will result in an ' s, [( w) }3 W8 T" Eincorrect titration. The fading end-point does not occur at the second / o) ?3 a% ]! g* O. p$ W3 v5 {end-point.) ' n# t, X' I9 X" v0 E' FAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a ' |5 ?6 m! @) h z: w6 Hstream of running water. Titrate this solution, using the zinc sulfate 7 U! G+ f9 y5 @) nsolution as titrant, to the same fugitive yellow-brown or pink end-point. L5 q0 {4 ^) A+ u* G8 ^3 X
as described above.# d" n/ B8 r u1 V/ C6 j, D
Calculate the titre T of zinc sulfate solution by the formula: + s1 Q1 V' M# H( x0 G# \$ dT = 18.896 W / V ]4 n6 n+ R5 B% S1 qwhere - ]3 V: f- ?( m; V8 W; [6 NT is the mass (mg) of Al2O3 per ml of zinc sulfate solution! C% `, f- @# B; @8 \1 e
W is the mass (g) of aluminium wire : z! \9 J2 Z9 Q$ q zV is the ml of the zinc sulfate solution consumed in the) R" F6 @4 z( i" a6 s
second titration * K1 d4 u z0 m& P/ m- a3 ? d18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and 5 Z6 W+ }+ q* xR is the ratio of the formula weight of aluminium oxide to& L9 A0 ]3 Z- z6 |, z
that of elemental aluminium. 8 u# P' U1 @( O$ lSample Solution A2 Y- L; ?6 P9 N3 q1 O
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica + ?9 W& D$ \3 ~. C5 L4 Z7 q5 eglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).- e$ R$ P- Q7 M& |/ a _
(Note: Do not use more sodium bisulfate than specified, as an excess' _% L' J) _5 G+ G* U( c
concentration of salt will interfere with the EDTA titration later on in the 2 G* b) u, f7 N! W, M7 _2 k/ X; Uprocedure.) Begin heating the flask at low heat on a hot plate, and' s* d8 p( }: `
then gradually raise the temperature until full heat is reached. 8 ?1 c6 Z% v F9 V c(Caution: perform this procedure in a well ventilated area. ) When 5 h: A) p- L% e5 \spattering has stopped and light fumes of SO3 appear, heat in the full 8 r+ e& C1 K) sflame of a Meeker burner, with the flask tilted so that the fusion of the6 ~ Y" _3 K, Z- f# Z# h
sample and sodium bisulfate is concentrated at one end of the flask.7 H- R, B8 n I0 Z+ H8 ~
Swirl constantly until the melt is clear (except for silica content), but' C* Y# ~% v2 X5 m; k1 ]
guard against prolonged heating to avoid precipitation of titanium + I0 @% n# e3 L1 ` v& Udioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until 6 i) k) s- ? zthe mass has dissolved and a clear solution results. Cool, and dilute to ) B; D2 u; i0 O$ c/ ?; a7 B120 ml with water. Introduce a magnetic stir bar into the flask.4 h+ m, M1 L' O
Sample Solution B/ Q+ l1 \6 g, P) K w1 q2 J
Prepare 200 ml of an approximately 6.25 M solution of sodium 1 j y4 A' Z, b3 Xhydroxide. Add 65 ml of this solution to Sample Solution A, while5 |3 M4 j; h: d! m+ u. E$ B) ?
stirring with the magnetic stirrer; pour the remaining 135 ml of the * \1 M0 e3 ~$ m" V1 A! Oalkali solution into a 500-ml volumetric flask. / z. m3 U( y" x- d. USlowly, with constant stirring, add the sample mixture to the alkali 4 z# l1 d& z! ?; A6 |3 [0 h; xsolution in the 500-ml volumetric flask; dilute to volume with water, ( p$ w' `; d7 sand mix. (Note: If the procedure is delayed at this point for more than I0 Q4 ?! u5 Y
2 hours, store the contents of the volumetric flask in a polyethylene! O1 ]7 G3 S+ }. I8 Z
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),* y ~7 v7 M" ]' _& c0 F! X7 U
then filter the supernatant liquid through a very fine filter paper. Label : V9 q* S, Y; W) S/ gthe filtrate Sample Solution B.& U6 H5 ^; x1 f8 E0 l9 h
Sample Solution C # R+ D7 f7 G1 [& F2 wTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer5 P. |( @% @" g. t. `' m; Y
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid + p! h9 {5 j+ j ?% _, S5 s+ |solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02 - I8 h$ R! u" [8 }+ w, H8 R7 P! vM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is0 h& J4 X1 V8 ?
known, calculate the optimum volume of EDTA solution to be added & x3 `9 v: l8 q" tby the formula: (4 x % Al2O3) + 5.] : C& M* C- m) e% F: Z, X) U6 ]- H$ tAdd, dropwise, ammonia solution (1 in 5) until the colour is just 1 ]; c) H- k8 ^& b; ocompletely changed from red to orange-yellow. Then add10 ml each 4 f' n V4 M0 a: S" ]of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to I6 n; J7 b" G+ J6 Z' q7 @1 sroom temperature in a stream of running water, add 3 drops of xylenol6 Q. I, i0 W, p
orange TS, and mix. If the solution is purple, yellow-brown, or pink,/ H1 Q2 V6 \. d5 y1 O+ u
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired 1 S x3 @7 C) K1 |pH, a pink colour indicates that not enough of the EDTA solution has * D& w# ^9 N+ G& y1 j; A4 J' @1 Nbeen added, in which case, discard the solution and repeat this" W: F" y8 K( W& Z
procedure with another 100 ml of Sample Solution B, using 50 ml,: @) ]- V3 T; c$ u
rather than 25 ml, of 0.02 M disodium EDTA. ( i' H$ w% G. G; g& ^8 Q6 F8 VProcedure$ A, g: |; i* l. u2 c4 @1 m/ B/ e
Using the standardized zinc sulfate solution as titrant, titrate Sample & j3 v2 e, n' v/ _3 \6 I5 qSolution C to the first yellow-brown or pink end-point that persists for J5 H9 B# [) ?+ r: n5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first1 k# ^$ |% g- v$ j/ H2 C$ Q9 H
titration should require more than 8 ml of titrant, but for more accurate $ f# ^4 S+ e# n2 K& {work a titration of 10-15 ml is desirable.. U; J% V- o3 ?! L4 j3 ?7 `
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5 : n- Q9 X% V6 Mmin, and cool in a stream of running water. Titrate this solution, using * S2 N; K# H" t6 f: i. Athe standardized zinc sulfate solution as titrant, to the same fugitive * e# |4 {/ w: ^+ u8 Zyellow-brown or pink end-point as described above. 9 k7 w; }' _# O( P& ~Calculation: & O" |% j$ e6 I4 bCalculate the percentage of aluminium oxide (Al2O3) in the sample" f o# d$ x0 w6 I+ i, s- ?
taken by the formula: . \: P5 k( [# r) V! l% Al2O3 = 100 × (0.005VT)/S: h2 _. h. i, f
where - L. D8 n& C, F1 ~' BV is the number of ml of 0.01 N zinc sulfate consumed in / x8 q8 V; ^5 k8 W* ?the second titration,% W4 k( A$ p3 `2 G) u" A3 {2 \
T is the titre of the zinc sulfate solution, 5 D4 k; x; C9 x% e" BS is the mass (g) of the sample taken, and. h& E! H7 H0 q
0.005 = 500 ml / (1000mg/g × 100 ml). , k8 R& n8 t% x& ~) b2 i! RSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica ! Y8 Z4 [3 ~4 _$ d! V* J2 C& Iglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O). 0 a/ P" I1 p1 W m, @& O# HHeat gently over a Meeker burner, while swirling the flask, until + `1 w$ g% ~ N9 \ Y; Odecomposition and fusion are complete and the melt is clear, except , U& U2 H5 A0 Y5 ]! O) Q/ S* Ofor the silica content, and then cool. (Caution: Do not overheat the . y1 E8 ? U' \; V# Kcontents of the flask at the beginning, and heat cautiously during ' g8 [& @3 @( Ifusion to avoid spattering.)' s+ ~; V1 p( v* @& k
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat $ M9 S: a. y+ F4 D0 p0 [9 _% t7 v& m Pcarefully and slowly until the melt is dissolved. Cool, and carefully add- W- x, T) j! m2 D4 _3 W
150 ml of water by pouring very small portions down the sides of the 4 P! i1 F+ G- b1 N/ ]7 v- ~flask, with frequent swirling to avoid over-heating and spattering. Allow: a" S6 K6 T& a" ~/ @2 ]
the contents of the flask to cool, and filter through fine ashless filter ( l/ ]* a2 x9 Q# @, Q7 y" `' dpaper, using a 60 degree gravity funnel. Rinse out all the silica from* w+ I# w; Y! S! P. E4 j, @
the flask onto the filter paper with sulfuric acid solution (1 in 10). + T7 L4 I+ `1 F# E1 FTransfer the filter paper and its contents into a platinum crucible, dry in, E; k1 p. @2 i8 b) _1 ^
an oven at 1200, and heat the partly covered crucible over a Bunsen( g* c8 ]7 M8 T3 g3 t
burner. To prevent flaming of the filter paper, first heat the cover from ; \" g9 L! K aabove, and then the crucible from below.; T9 f# ^2 |9 Y( O& B3 D1 m4 c
When the filter paper is consumed, transfer the crucible to a muffle) Z$ |: x& P* O' l {) O
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and 7 P! `, m: k. D2 \! W+ k; pweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated 6 q- X+ u; O J+ h3 H3 M8 P9 ahydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first$ m/ n* S, C: h! H+ j! w
on a low-heat hot plate (to remove the HF) and then over a Bunsen ' }; b* ]! R) h; S" y4 v8 A$ s" Rburner (to remove the H2SO4). Take precautions to avoid spattering,- Y1 }( b* m5 [7 L; @
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a 4 |6 O% `! ?# p4 ]+ F/ Fdesiccator, and weigh again. Record the difference between the two 5 u+ {; F9 N4 a c4 [weights as the content of SiO2 in the sample.$ d" |# n7 r# a L
METHOD OF ASSAY8 x$ d4 m6 l j6 a
Accurately weigh about 150 mg of the sample, previously dried at 105o 4 c8 p' R0 g+ _5 k0 ffor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water 3 M7 |, h" @$ k f6 Xand shake until a homogeneous, milky suspension is obtained. Add 30 8 h. [- F* g; Z! P3 C, q3 ^! pml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially$ J N- l" i, K, g1 _3 E- g
heat gently, then heat strongly until a clear solution is obtained. Cool, ' U" d1 s I7 u/ M, @then cautiously dilute with 120 ml of water and 40 ml of hydrochloric # N1 K T+ t5 K' h" Lacid, and stir. Add 3 g of aluminium metal, and immediately insert a' d' t) H8 s0 X
rubber stopper fitted with a U-shaped glass tube while immersing the 8 v2 [. T4 P8 o. c( bother end of the U-tube into a saturated solution of sodium7 d& k) a: Z. x# }- Z
bicarbonate contained in a 500-ml wide-mouth bottle, and generate* B( A# y+ c$ q. q4 a3 F; |4 R4 e
hydrogen. Allow to stand for a few minutes after the aluminium metal, L, S/ d5 d- f6 S: e6 u
has dissolved completely to produce a transparent purple solution." D2 s3 x* I6 Q# Q
Cool to below 50o in running water, and remove the rubber stopper# x; j0 ?7 D6 q0 B& V! w
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate 1 W% j$ K+ k: x+ g- ~# P: ksolution as an indicator, and immediately titrate with 0.2 N ferric 7 y! g' y* T3 ?, @( W6 k. h \ammonium sulfate until a faint brown colour that persists for 30( F9 a! d8 a b. U3 i5 y* ~
seconds is obtained. Perform a blank determination and make any! @9 Q5 T S/ ^
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is' m S+ P& N, p9 i
equivalent to 7.990 mg of TiO2. / a. @) o/ l5 [* N$ F