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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) 9 Y/ N0 \- w9 \/ }+ I% ^
6 H5 D  l3 k: y) o
1 x/ r9 \  r- |  {4 j
CAC关于二氧化钛(钛白粉)的使用规定: h- O( t" Y6 w# u' w
GSFA Online
' U' t- a& h+ m! rFood Additive Details
( q4 @4 U; e6 G, J( e# |2 DTitanium Dioxide (171)$ ^* B5 w" {1 A
Number Food Category  
! Q" u. I/ y, J7 V  01.1.2 Dairy-based drinks, flavoured and/or fermented (e.g., chocolate milk, cocoa, eggnog, drinking yoghurt, whey-based drinks)  ( v# ^: ]/ B1 `* z0 z
  01.3 Condensed milk and analogues (plain)  6 y6 @5 ?; |3 r% j% ]9 w
  01.4.3 Clotted cream (plain)  
6 z( y+ r' l" W+ x7 U( ^  01.4.4 Cream analogues  
: X. f+ ]2 r+ E' I- S) T8 g+ [% n  01.5 Milk powder and cream powder and powder analogues (plain)    Z9 x/ N6 g+ p: K# a
  01.6 Cheese and analogues  - J; d9 Q- F. e
  01.7 Dairy-based desserts (e.g., pudding, fruit or flavoured yoghurt)  
! x8 M4 P6 K9 P3 e/ G7 `3 R2 c  01.8 Whey and whey products, excluding whey cheeses  . l. l/ }7 o2 e4 o; `
  02.2.1.2 Margarine and similar products   % ~1 y: r* W5 A, }' }% B6 f
  02.2.1.3 Blends of butter and margarine  ' T  k$ W* j; R4 A9 f3 C1 `
  02.2.2 Emulsions containing less than 80% fat   
" w- F3 Y+ @* X# ?6 ]  02.3 Fat emulsions maily of type oil-in-water, including mixed and/or flavoured products based on fat emulsions   
8 Y, o  s2 A# \$ }3 l( W  02.4 Fat-based desserts excluding dairy-based dessert products of food category 01.7  6 o! ]! T2 I# P: S/ S
  03.0 Edible ices, including sherbet and sorbet  
& S2 S4 q4 w4 x( s! H  04.1.2 Processed fruit  7 `+ V0 n' P" Q
  04.2.2.2 Dried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweeds, and nuts and seeds  
" R4 L# _0 {" ]& F  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 L5 T" M& q; {4 _0 c  c  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  
1 H4 n6 Z0 M, x4 v# {7 e  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)  ) e1 i3 h$ B( o5 Y3 D1 g& f& v
  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  
* o5 B7 U4 f. R" _& G* b2 r  04.2.2.8 Cooked or fried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  5 @: J; h5 }# y
  05.0 Confectionery  
$ k; }' X8 ^+ J" N$ E  06.3 Breakfast cereals, including rolled oats  
/ Y3 r+ v0 L# e! R  06.4.3 Pre-cooked pastas and noodles and like products  : K. q' _, O' P  Y+ K7 Q) q! |
  06.5 Cereal and starch based desserts (e.g., rice pudding, tapioca pudding)  
3 r! e  ^; [. V, G; Q5 _  06.6 Batters (e.g., for breading or batters for fish or poultry)  
) ~) V8 w5 T' M) m7 i1 ?2 s8 C4 m  06.7 Pre-cooked or processed rice products, including rice cakes (Oriental type only)  ' l3 \- h# u7 d- |
  06.8 Soybean products (excluding soybean products of food category 12.9 and fermented soybean products of food category 12.10)  0 x7 D6 P9 N( x: w
  07.0 Bakery wares  
5 X1 A0 U* s3 I# f. E- o  08.2 Processed meat, poultry, and game products in whole pieces or cuts  7 r3 K1 c" r. H( p" i
  08.3 Processed comminuted meat, poultry, and game products  
; T  D! p( r7 h7 o3 x  08.4 Edible casings (e.g., sausage casings)  
7 z8 E: `3 F4 p) k; K$ c  09.3 Semi-preserved fish and fish products, including mollusks, crustaceans, and echinoderms  
8 J5 t6 k. @% Y( k) l4 B; r  09.4 Fully preserved, including canned or fermented fish and fish products, including mollusks, crustaceans, and echinoderms  ' t' M  b8 t% n, v- |2 c, Q
  10.2.3 Dried and/or heat coagulated egg products  
- k& w9 |9 r5 J+ w2 F3 V4 [! u  10.3 Preserved eggs, including alkaline, salted, and canned eggs  
  n* e; r+ r+ a6 A& Z' S9 n  10.4 Egg-based desserts (e.g., custard)  ) W! k" e7 O7 X" q2 I
  11.6 Table-top sweeteners, including those containing high-intensity sweeteners  
1 O; i) E# o1 R# T$ r  12.2.2 Seasonings and condiments    b! a6 C1 Y0 |3 x+ _' H- [0 W* f, `
  12.3 Vinegars  & [0 t' a6 H+ u# t  m& h
  12.4 Mustards  6 [6 m) h6 G- Y2 I! D8 n. R
  12.5 Soups and broths  ) T9 m- q) A( a; U0 |: v" {
  12.6 Sauces and like products  
  o% E$ y# p7 \& t* Y9 f- k9 B6 s  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  ; `2 P3 g: I$ b/ t
  12.8 Yeast and like products  
! c8 K0 G% f0 e# M. n5 [- S  12.9 Protein products  9 h" @1 u2 ?0 u0 W2 y5 d
  12.10 Fermented soybean products  ; Z; X; S1 G6 N: e% a" i
  13.3 Dietetic foods intended for special medical purposes (excluding products of food category 13.1)  4 F, J3 L. J8 \0 q) n
  13.4 Dietetic formulae for slimming purposes and weight reduction  ! h# v# }7 T! m- n
  13.5 Dietetic foods (e.g., supplementary foods for dietary use) excluding products of food categories 13.1 - 13.4 and 13.6  
. l4 U) ^, h& V6 }; |- c1 G9 W8 I' a- O  13.6 Food supplements  
3 ?' L! p+ O+ h5 l) K7 W  14.1.1.2 Table waters and soda waters  
+ o+ S% C- _3 C) E; i  14.1.4 Water-based flavoured drinks, including "sport," "energy," or "electrolyte" drinks and particulated drinks  
6 J  b; a( \6 L7 _& q  14.2.1 Beer and malt beverages  
' m' l, w1 o( Y, Z4 K; s  14.2.2 Cider and perry  
* K6 ?! m  t  P0 X5 C1 G. v  14.2.4 Wines (other than grape)  
$ B+ o: r: \1 R, `- X! d' g  14.2.5 Mead  7 d1 O% ?  `8 c
  14.2.6 Distilled spirituous beverages containing more than 15% alcohol  , w: v8 u/ Y, o9 Y2 z8 H; W
  14.2.7 Aromatized alcoholic beverages (e.g., beer, wine and spirituous cooler-type beverages, low alcoholic refreshers)  
9 B. s7 Q2 L. i( M& h  15.0 Ready-to-eat savouries  ' K* a' ]$ G1 |5 i0 X
  16.0 Composite foods - foods that could not be placed in categories 01 – 15, l" I7 A# t6 A3 ]  U8 i

' r5 L' v; u: [$ j5 n0 Q  Y& c( C: ^3 o$ A8 z
部分译文:
8 W% D5 Y3 B, f0 F. V
. c1 b7 D0 h8 ^7 c食品添加剂通用规则/ z9 K* D. Y5 k5 N1 P
食品添加剂
2 ?) w0 Q' ~5 Y8 {; ~! A' g7 R  O                    二氧化钛(171)4 n) r4 Z  h( ?, X
食品类别:3 K# T" `) I  _; F1 P
06.3 早餐谷类,包括燕麦片
3 N" V" U' \1 ^- L0 E5 S: z06.4.3面条及类似产品
  W9 c( |4 J! Q2 ?$ @" I# ]06.5 谷类,淀粉甜点(包括:米粉布丁,木薯布丁)
7 y, ^2 M' w, j6 i, {# \06.6 面团
7 K4 z; Q# p$ _! u+ d; k06.7 预煮的或加工的米产品,包括年糕(只包括中式的)06.8 Soybean products
9 G9 y' v: {$ x: w4 W* A07.0 烘焙类
7 A2 r; Z  V$ F6 B$ }8 W& x07.1 面包,普通烘焙类,以及其混合物
9 y' D' [& R& t0 e" J& v& W& p6 G07.1.1 面包,面包卷$ z+ _& R7 S$ ~0 Q3 e, A
07.1.1.1 酵母发酵面包及特殊面包
2 h9 t' Y. v. }0 S. X07.1.1.2 苏打面包0 e% x5 d7 c" {! X% r
2 H2 Q1 ^- q) R" ^5 x9 G. p! I3 h

; P' N+ l& S* I9 x, W3 `
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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); I% i* D5 c- x- q5 a+ c

; j  H+ V. i& O0 {; oJECFA关于二氧化钛(钛白粉)的结论5 \0 n3 y  |% \% I% N2 i

$ Y& K- x3 ~. i# I3 b摘要: 2006年JECFA关于二氧化钛的结论
9 _" S1 b4 R# N) Y7 T* W% e, ?4 {ADI值:不作限制。' B5 v. q* G! v. F
功能:着色剂
/ ]1 V0 t; W* l2 R3 E3 P: D7 K# E8 A3 {# D3 U7 V
TITANIUM DIOXIDE
, n- }/ Q, i, K4 E% v' W( z- ?4 OPrepared at the 67th JECFA (2006) and published in FAO JECFA
0 Y& P0 G4 b  R. N) J8 ?Monographs 3 (2006), superseding specifications prepared at the 63rd6 c5 `$ d/ t# t7 Y4 c
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
* m  N/ H+ X9 z3 ^) t9 x; gCombined Compendium of Food Additive Specifications, FAO JECFA5 c# I# s% f3 Q; y
Monographs 1 (2005). An ADI “not limited” was established at the 13th$ t; a% V+ e/ u  c: ?: X; D
JECFA (1969).4 e$ U  Z* Q6 g! d
SYNONYMS
, l/ H) p/ g# D  z* l' x& K# QTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171. j- u! ]5 @" k/ a$ ^9 D6 `2 w
DEFINITION
5 G  |9 G* |) z( y  ATitanium dioxide is produced by either the sulfate or the chloride8 R$ \) s' y, t: D- {3 E
process. Processing conditions determine the form (anatase or rutile
. i3 H; m2 R, i& W( ?9 i7 Zstructure) of the final product.
" P' b& {0 |4 }3 FIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)4 |2 ?+ D) T( Y! P+ n
or ilmenite and titanium slag. After a series of purification steps, the
& b4 q' R; O) `! Hisolated titanium dioxide is finally washed with water, calcined, and! Q" o8 w0 y8 U7 z3 y4 c: `
micronized.
% {  n3 ]+ A. M( tIn the chloride process, chlorine gas is reacted with a titaniumcontaining6 ~5 H$ `: @7 i7 n
mineral under reducing conditions to form anhydrous1 N& P6 |# G2 M8 }
titanium tetrachloride, which is subsequently purified and converted to# E1 @2 P" [9 s( X: d
titanium dioxide either by direct thermal oxidation or by reaction with. h& o4 M2 H8 a8 r) ]6 [
steam in the vapour phase. Alternatively, concentrated hydrochloric
' z: G4 F! [8 ^( [. kacid can be reacted with the titanium-containing mineral to form a
/ d1 G9 F0 G) U1 E3 O7 ]' o3 ksolution of titanium tetrachloride, which is then further purified and- [" F! Y3 N+ }: b; H
converted to titanium dioxide by hydrolysis. The titanium dioxide is
* g! z: z# z) g2 f% z+ jfiltered, washed, and calcined.
  h5 ?+ w1 t* W6 j; V! y* _6 NCommercial titanium dioxide may be coated with small amounts of( @$ J6 p9 a: [8 R8 H. m
alumina and/or silica to improve the technological properties of the( m+ t+ x2 x0 {- e, q' d
product.( @% S& ?* I: A! E
C.A.S. number 13463-67-7
% p( f* }0 |7 A9 JChemical formula TiO2
) S% h$ d6 R, \3 NFormula weight& _9 x) T% Y/ Q/ N7 o
79.88
1 O) d8 t$ u$ UAssay3 Y/ m- M3 b5 z; [5 _" z' t
Not less than 99.0% on the dried basis (on an aluminium oxide and
& V# N  ~$ i+ F2 D  nsilicon dioxide-free basis)
: U, |9 y6 \+ j  |- g1 k1 y: HDESCRIPTION
/ {7 u) y2 o+ e  u( O2 RWhite to slightly coloured powder$ V  s( `/ G0 l3 H9 e
FUNCTIONAL USES
& S6 Q4 f* X  Q  j! NColour
2 G1 S6 l: y; u, w' ], @8 W9 ECHARACTERISTICS* P4 s' l! ?* J4 X" c) x  o
IDENTIFICATION
' @- O% Y9 X4 E/ |Solubility (Vol. 4)
9 O% Z8 }# _5 P# m' O+ x, @6 RInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic6 s3 _: O" m2 w' D! [5 l
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
5 K+ {5 U5 v$ i8 }2 isulfuric acid.4 u" V4 ~  Q* g0 \  K) S
Colour reaction, m3 T6 U  B4 V. T6 f# ]
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of/ W6 ]6 @0 c: f$ i) T
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
7 }% c3 y& P9 I  T  qwater and filter. To 5 ml of this clear filtrate, add a few drops of
( m6 G5 j* V  G6 B% P' v% yhydrogen peroxide; an orange-red colour appears immediately.* l7 D9 O2 Y6 x: J; g* Y! u
PURITY
7 Y- N' H4 @+ ]9 LLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)7 j9 E6 R$ x$ H, ~% ~; f* p# f" u
Loss on ignition (Vol. 4)
. ~4 u& S+ y+ QNot more than 1.0% (800o) on the dried basis
2 b* c/ `7 e; p5 ]* t) A, G" wAluminium oxide and/or
9 h5 j3 z& P3 Y; _3 F. L' ]silicon dioxide
0 Y; m& {  Z2 a. WNot more than 2%, either singly or combined7 O: Q( z7 v8 n. \  l
See descriptions under TESTS. c3 A6 |* ]2 J0 b% f6 J7 R
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
3 R3 C- y& W  B6 |alumina or silica.+ y9 j; q8 C" H1 j# T! r: T/ s
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
; |! Z7 J" K* M) `& Q% Cplace on a steam bath for 30 min with occasional stirring. Filter7 J( }) n& ~5 T) J: f$ L, y
through a Gooch crucible fitted with a glass fibre filter paper. Wash
) }3 K' n7 a, i8 Mwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the( a, J; v* ~3 `, u* O2 z& \0 X
combined filtrate and washings to dryness, and ignite at a dull red( [% h( R/ x5 t# B7 {# @
heat to constant weight.
+ _! ?6 s# i7 J9 a# P1 j7 C9 n  z' \* `" oWater-soluble matter( x1 K2 Q( c6 l
(Vol. 4)7 x) Q6 s0 _' s4 V2 V
Not more than 0.5%
' _0 [  V- V, {* k1 dProceed as directed under acid-soluble substances (above), using
! r5 x/ y) c9 \5 q; I$ z2 Mwater in place of 0.5 N hydrochloric acid.
% h  G" |* A- h0 A2 M( W& XImpurities soluble in 0.5 N
% `/ w- O5 u# M' Khydrochloric acid, Z# w' G$ E! L4 p5 j2 T: ]
Antimony Not more than 2 mg/kg) u4 g% J7 A, c* d( ]/ z- W' Y: \
See description under TESTS, F; Z8 G$ u- e- m
Arsenic Not more than 1 mg/kg
  X6 C" `) ~0 o: F0 s0 ]7 ~, P+ KSee description under TESTS
& S* D$ y0 p: w; ^4 Z7 g( FCadmium Not more than 1 mg/kg& l* J& m; p/ v/ `2 S7 S6 B. w" D
See description under TESTS
- a8 F: r3 V& ]$ D. bLead  h8 V+ {( Y7 G; K2 z
Not more than 10 mg/kg+ z2 N7 u4 }. \3 a  S4 z$ f1 r
See description under TESTS
, s4 M' C; ^7 X) V. g! |Mercury (Vol. 4) Not more than 1 mg/kg
& g( V2 d  U6 i3 q7 {, [  U" ?Determine using the cold vapour atomic absorption technique. Select a
/ n# V. `8 g! q& R' Fsample size appropriate to the specified level3 k. @6 }$ p& M9 W  n
TESTS% X6 ~6 S$ G1 M2 u) r8 {& _  N
PURITY TESTS: f% X3 f8 n" ~% U5 c4 h. O
Impurities soluble in 0.5 N! j) b( t5 [1 B( _: N, Z
hydrochloric acid
2 C1 _7 i  h- W# C, o2 w' }Antimony, arsenic,
# U1 y: J/ T9 w4 I) n9 Q: a8 t# K! k# Kcadmium and lead' S' w1 t4 s  f" d9 t
(Vol.4)2 C0 B" q0 i8 \% O* L
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N4 q! G; n+ n/ N" [1 K$ Z9 ]
hydrochloric acid, cover with a watch glass, and heat to boiling on a" f  S* ?, Z4 h- n/ `
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
  Y$ _1 p6 C  x% U' Jcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved2 b) ^. i1 ?8 d; T1 ~
material settles. Decant the supernatant extract through a Whatman
# S' m/ C: Y9 N: xNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml" L" B  C: L/ Z! z4 Z
volumetric flask and retaining as much as possible of the undissolved6 E) t, l% ]/ `0 T3 ~+ F4 A
material in the centrifuge bottle. Add 10 ml of hot water to the original
7 e. y7 l) |1 h; E6 d# m3 y! Qbeaker, washing off the watch glass with the water, and pour the& ^# y& `( S+ T# ~9 h
contents into the centrifuge bottle. Form a slurry, using a glass stirring$ j) x4 w# P. i( V& o. S8 [. P; E
rod, and centrifuge. Decant through the same filter paper, and collect/ ?# `  O+ q$ d
the washings in the volumetric flask containing the initial extract.
& \& ~: Q4 a" u4 s% XRepeat the entire washing process two more times. Finally, wash the0 ^3 c8 U) Q- |+ |) v: l
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
6 e& T9 Z. S0 w2 x/ I6 {9 qto room temperature, dilute to volume with water, and mix.0 D( d4 B( h5 L5 c
Determine antimony, cadmium, and lead using an AAS/ICP-AES
9 d6 h2 o  y! X: w+ R% Y" y# Atechnique appropriate to the specified level. Determine arsenic using the5 o$ o( g3 B* k# b9 |
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using1 V; d& t* k  I& h
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than: C' D& ~/ t1 a# A. K# @  u
1 g. The selection of sample size and method of sample preparation% Y8 K+ G8 G- V7 u
may be based on the principles of the methods described in Volume 4.
: k" W! F, k4 ?6 I2 y2 o3 c2 L  UAluminium oxide Reagents and sample solutions7 a( r9 R' l! S8 N
0.01 N Zinc Sulfate
4 Q* x8 O3 I6 Z# u3 iDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to3 M& s% K$ t  b2 X
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg4 x8 Q' N# \3 J3 Z  J
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
& Q$ `  t! C( T- Jconcentrated hydrochloric acid, heating gently to effect solution, then# H' m1 ?$ s( E/ R, c
transfer the solution into a 1000-ml volumetric flask, dilute to volume: P- U% `0 `' R! z
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
% u& ^" M& M( x) ~ml Erlenmeyer flask containing 90 ml of water and 3 ml of
. ^! w: q" Z6 ?0 R+ ^concentrated hydrochloric acid, add 1 drop of methyl orange TS and$ I  f: K6 E+ W2 S3 X2 `
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
4 }1 ]' R0 t5 L5 sdropwise, ammonia solution (1 in 5) until the colour is just completely( G% e5 X5 m; m# k; c
changed from red to orange-yellow. Then, add:. [" ^% F/ L5 U0 k  L  |* H+ U' \
(a): 10 ml of ammonium acetate buffer solution (77 g of4 B; i! c  p# Y9 {# _
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
, x3 f! o, Z# @4 r1000 ml with water) and
. N/ k9 M7 Y* u: S0 |(b): 10 ml of diammonium hydrogen phosphate solution (150 g2 x3 s  z% @1 X9 d/ c- U
of diammonium hydrogen phosphate in 700 ml of water,/ J/ e+ K5 E7 w! e
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
+ g2 i0 C, T1 n+ Y& L+ j% a) vthen dilute to 1000 ml with water).
; S$ y  ~2 u; ^0 eBoil the solution for 5 min, cool it quickly to room temperature in a
- s3 V$ C+ b3 S& Ystream of running water, add 3 drops of xylenol orange TS, and mix., k/ V& U5 _1 B+ [1 C  R
Using the zinc sulfate solution as titrant, titrate the solution to the first5 y' b& |/ X0 V2 S
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
, g( b2 M0 N7 eThis titration should be performed quickly near the end-point by0 k6 F  H0 g5 {2 f3 T0 d+ _
adding rapidly 0.2 ml increments of the titrant until the first colour
+ B# C( c9 p3 h, h, `. \1 ^change occurs; although the colour will fade in 5-10 sec, it is the true
  j6 X- p8 M9 J: ~end-point. Failure to observe the first colour change will result in an
- x# h/ F. b" e8 D, aincorrect titration. The fading end-point does not occur at the second& g# W7 P( R) F2 Q% D/ E! d
end-point.)4 x) g" ]/ O' p! i+ q: |/ ?! ]! {
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a/ s3 T2 F0 e& D5 J+ g
stream of running water. Titrate this solution, using the zinc sulfate) k# U  I) C. \
solution as titrant, to the same fugitive yellow-brown or pink end-point* m: E5 K1 T  q) ], ?! O
as described above.
1 S' l1 }: S2 ]Calculate the titre T of zinc sulfate solution by the formula:
- N1 }8 V% }! X2 G! a8 xT = 18.896 W / V/ G: y* d  A4 @# Z  N# [4 H' t
where; N8 G, M2 L7 V: @& v* W. h
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution) V/ W* W3 O4 B- m
W is the mass (g) of aluminium wire% ]/ N% r1 p" C* W- Z! y3 _! ?
V is the ml of the zinc sulfate solution consumed in the
1 O# q8 j! q# E. `9 b, Isecond titration
! c* t# Q+ x+ `18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
* P# Z9 A  `7 L- x# l  mR is the ratio of the formula weight of aluminium oxide to
. T$ n  O7 m7 N5 `that of elemental aluminium.8 ?- Z8 l( v) q9 e1 s2 Y5 N
Sample Solution A& _% A/ C) L) k& y( @7 }% n
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
9 s/ p- }9 o: t5 @glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
) q, o1 ?( S- X(Note: Do not use more sodium bisulfate than specified, as an excess
+ M5 N8 w1 ^5 m, v8 hconcentration of salt will interfere with the EDTA titration later on in the" |# u; O8 L2 i/ `+ q
procedure.) Begin heating the flask at low heat on a hot plate, and. z* }1 S; k2 b$ E2 \7 e
then gradually raise the temperature until full heat is reached.
1 |# k& X. Z( i" H* `, b, F(Caution: perform this procedure in a well ventilated area. ) When; L2 K* o5 y6 y2 T8 G5 m0 x5 o
spattering has stopped and light fumes of SO3 appear, heat in the full% O" K9 I0 i! q4 K4 N# T; [
flame of a Meeker burner, with the flask tilted so that the fusion of the
8 o6 a0 ~- x7 hsample and sodium bisulfate is concentrated at one end of the flask.  I% T! B0 p0 V  x& _1 m) j8 l
Swirl constantly until the melt is clear (except for silica content), but
# Q: Y" S% j3 L8 U5 gguard against prolonged heating to avoid precipitation of titanium
* Q" I% c4 P$ idioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
1 O, l, k& \: x# bthe mass has dissolved and a clear solution results. Cool, and dilute to
- `" Y) t( {! d; o9 U120 ml with water. Introduce a magnetic stir bar into the flask.. G* B5 y, a+ O5 @. y
Sample Solution B
; U7 a4 {3 g3 \/ |$ C: V' D1 X& Q. yPrepare 200 ml of an approximately 6.25 M solution of sodium5 Y- j0 |, j; R9 ~2 f( U
hydroxide. Add 65 ml of this solution to Sample Solution A, while
6 @) w' u) |6 ^) X& K" Rstirring with the magnetic stirrer; pour the remaining 135 ml of the
1 L; G% Y! N0 G$ e. Nalkali solution into a 500-ml volumetric flask.3 i- r  j  ^- A1 x1 @* D7 i
Slowly, with constant stirring, add the sample mixture to the alkali
; {" m* F2 I! ]- t+ w; J" ?3 |, rsolution in the 500-ml volumetric flask; dilute to volume with water,4 \' ^' W( R' s, [! [; H
and mix. (Note: If the procedure is delayed at this point for more than
* I0 k/ X+ H$ o+ M! ]$ G: _" T. |7 K4 d2 hours, store the contents of the volumetric flask in a polyethylene$ V; j2 E6 L. b6 ], f2 Q& F3 G" n
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),& Y& b7 f5 Z* u
then filter the supernatant liquid through a very fine filter paper. Label0 }1 e6 V% X1 B6 f+ p; o
the filtrate Sample Solution B.
  L, p/ l8 M% l0 m$ X6 F- bSample Solution C
  W. p; k9 q+ S: f/ I; lTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
8 u& P! ?6 Z5 p+ [flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid" F* {6 t1 I  w8 y% i2 q
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
! C- I' G1 W- J7 Y, x" DM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
3 q* x6 u( j, `: F- yknown, calculate the optimum volume of EDTA solution to be added
/ W7 V% J& p" B. X+ |" Y( n4 Jby the formula: (4 x % Al2O3) + 5.]
( B* i" \/ ~* w! V; VAdd, dropwise, ammonia solution (1 in 5) until the colour is just
1 B$ ^. g3 E! `' X& j/ bcompletely changed from red to orange-yellow. Then add10 ml each
5 N- |" e$ @* F- |+ H( Xof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to" _6 Y/ M" s" W
room temperature in a stream of running water, add 3 drops of xylenol' [1 x+ X$ t: b; Y% l* ]. H
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
9 T6 u4 `- L1 ~. Sbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired7 h: d6 B1 f, L% N9 U
pH, a pink colour indicates that not enough of the EDTA solution has
) V  p4 g7 n- H0 Zbeen added, in which case, discard the solution and repeat this
. b$ h$ i7 P, R/ h$ c& xprocedure with another 100 ml of Sample Solution B, using 50 ml,
9 c$ R6 J7 _( R0 b) i( Erather than 25 ml, of 0.02 M disodium EDTA.
7 R2 M0 p+ g; K# U4 \* tProcedure
# e) Z& T8 p' p: O' {$ t6 sUsing the standardized zinc sulfate solution as titrant, titrate Sample
1 K$ @" ]* Y' W3 k: l! T% \) [* @Solution C to the first yellow-brown or pink end-point that persists for
1 \, |6 Q+ ~$ B- ?1 o/ V5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
/ |/ M0 E" v: p# v* ftitration should require more than 8 ml of titrant, but for more accurate9 T  s' Z$ y2 M% l( x0 V
work a titration of 10-15 ml is desirable.
8 f- E* q; M4 u) {8 a; A) aAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5- W0 s9 ?4 L6 v2 ~. p- r/ p4 R9 C: r
min, and cool in a stream of running water. Titrate this solution, using: [' {" K; y. |
the standardized zinc sulfate solution as titrant, to the same fugitive; d. O( \% p& L: e/ {3 z1 u
yellow-brown or pink end-point as described above.$ ]; t" w& Y4 N* @. i# _
Calculation:
3 H) F4 n+ m6 hCalculate the percentage of aluminium oxide (Al2O3) in the sample
$ G, ]$ C! ^& }8 X5 U  W" p' htaken by the formula:
8 f" k& p+ {3 _% Al2O3 = 100 × (0.005VT)/S
/ a2 O+ V3 E6 ?5 Pwhere
. ?9 O' L& f* U. {) yV is the number of ml of 0.01 N zinc sulfate consumed in
/ X) ^9 y, @% t9 @the second titration," Y3 }$ \; z$ ~0 L
T is the titre of the zinc sulfate solution,
0 S/ l$ g3 }* `4 ~# r  T, QS is the mass (g) of the sample taken, and
3 Z  |( H5 Z6 I2 L: e2 `+ ?0.005 = 500 ml / (1000mg/g × 100 ml).$ V6 g( \' W8 R* Y' ?
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica2 N1 P! @% D, i) G% ~+ o
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
' g, w9 ^+ j: {8 WHeat gently over a Meeker burner, while swirling the flask, until
& a9 _8 n9 c8 Ldecomposition and fusion are complete and the melt is clear, except8 r. o' S' G1 {* Y; h/ T/ V
for the silica content, and then cool. (Caution: Do not overheat the
+ T5 ~8 d  `1 J. Acontents of the flask at the beginning, and heat cautiously during- K! V( H7 F* o9 l$ w: L
fusion to avoid spattering.)% N2 Q8 c: K) k
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat5 ^7 r+ ]4 n6 z) R/ c8 Y: Y
carefully and slowly until the melt is dissolved. Cool, and carefully add
& V8 A, ~+ |7 V+ d  A+ C8 {0 Z150 ml of water by pouring very small portions down the sides of the
0 ?' Y0 `' Y. `3 x9 o* N% U& b- \flask, with frequent swirling to avoid over-heating and spattering. Allow
" Z  [- H+ v+ x: p4 uthe contents of the flask to cool, and filter through fine ashless filter7 Z" o' u2 I6 V
paper, using a 60 degree gravity funnel. Rinse out all the silica from% U' J, J( S6 C! Z% r. \9 E) k9 ^
the flask onto the filter paper with sulfuric acid solution (1 in 10).
; S' g8 V, d( ]2 X+ X  BTransfer the filter paper and its contents into a platinum crucible, dry in
' C& |5 g9 L# E/ R5 R! xan oven at 1200, and heat the partly covered crucible over a Bunsen
( A4 ?6 S8 @/ }% I* f1 b- Bburner. To prevent flaming of the filter paper, first heat the cover from
* G  h, z4 H4 Z9 Zabove, and then the crucible from below.9 @, O* I" R* l# V8 p: P
When the filter paper is consumed, transfer the crucible to a muffle- E( y+ d+ |+ z8 G8 d# f+ R; [
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and8 C$ i0 W& L  Q8 ?4 n9 ^4 Q" ?
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated7 d! X% X  h4 K: Z2 T
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
# V7 l( U" v! \7 Bon a low-heat hot plate (to remove the HF) and then over a Bunsen
4 X: f: a8 X- Dburner (to remove the H2SO4). Take precautions to avoid spattering,. ]0 _: g, l3 L0 n5 C) r
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a9 k( i" }9 E  Q
desiccator, and weigh again. Record the difference between the two+ b0 {" |7 x* h
weights as the content of SiO2 in the sample.. d4 I$ {$ T/ I5 _4 N( I7 h5 j
METHOD OF ASSAY
$ }7 N% U9 b2 AAccurately weigh about 150 mg of the sample, previously dried at 105o
) F  N0 e8 a- b+ n  A' E/ v7 wfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water6 h7 `) M2 Y2 C+ T# R5 r: l4 y1 p
and shake until a homogeneous, milky suspension is obtained. Add 30* c3 Y+ S7 F! M' I
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially2 G" r. Z) o3 d- q1 N5 w' q
heat gently, then heat strongly until a clear solution is obtained. Cool,7 X9 v: i+ c1 n$ ]& r
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
6 U/ I% m2 U% n# |5 Macid, and stir. Add 3 g of aluminium metal, and immediately insert a) S) Y, x3 G5 @( h& w# M- H- |
rubber stopper fitted with a U-shaped glass tube while immersing the
% L: ~; Q/ D0 G3 q6 ]0 @other end of the U-tube into a saturated solution of sodium
) S0 Y0 U$ V- ?# H4 h- Ibicarbonate contained in a 500-ml wide-mouth bottle, and generate7 p) V  ^& g: ?! s  z7 }
hydrogen. Allow to stand for a few minutes after the aluminium metal0 f% U1 X/ o' g9 ]8 ~4 @
has dissolved completely to produce a transparent purple solution.
7 i8 e9 {; p% pCool to below 50o in running water, and remove the rubber stopper8 G' M# _9 T8 A
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
6 r, E3 T" u2 t$ g& csolution as an indicator, and immediately titrate with 0.2 N ferric7 e9 z* d8 u) f3 A' ?3 T/ q
ammonium sulfate until a faint brown colour that persists for 30
3 F& x! B; s$ a7 C% U8 X% Y4 i5 {* lseconds is obtained. Perform a blank determination and make any
3 l; X; M, ?( m; Q% _2 b5 V7 Tnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
: F+ Y9 x- l8 n& kequivalent to 7.990 mg of TiO2.8 x6 f. c. R: r7 @+ q
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