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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)
# e: U& A( N2 F* W, v& w  j# I! Y5 w

% h/ m2 S6 Z5 C  D4 eCAC关于二氧化钛(钛白粉)的使用规定
7 k- x. l  z) e0 H0 tGSFA Online
. |4 Q0 ~/ y& |) D6 W9 `/ I2 H* @3 RFood Additive Details
5 M1 H3 v  T2 ?; C% eTitanium Dioxide (171)
, V: s: D+ q8 a9 W3 dNumber Food Category  
. ]. V* m( Y+ Q4 a* L! A, m  01.1.2 Dairy-based drinks, flavoured and/or fermented (e.g., chocolate milk, cocoa, eggnog, drinking yoghurt, whey-based drinks)  / L0 [5 Z) m: s+ {
  01.3 Condensed milk and analogues (plain)  
# Y2 ?, a5 B1 y8 n9 s7 ^  01.4.3 Clotted cream (plain)  
8 Z" Q  N' D9 T1 I8 E, ]  01.4.4 Cream analogues  
0 ^% P2 X5 h: b' J  |- d! H" ^! T8 d  01.5 Milk powder and cream powder and powder analogues (plain)  - @4 l2 I- c9 r: a  H
  01.6 Cheese and analogues  
+ k4 F$ F* ?/ V- t& A9 e9 _" t  01.7 Dairy-based desserts (e.g., pudding, fruit or flavoured yoghurt)  
* k  n. S* F' P9 f  L2 v& \# R  01.8 Whey and whey products, excluding whey cheeses  * w5 v6 v& t( f6 _3 s
  02.2.1.2 Margarine and similar products   
1 y. v' K+ h2 [5 V  02.2.1.3 Blends of butter and margarine  
" J( s% c$ I  j' ]& r  02.2.2 Emulsions containing less than 80% fat   ; D- m3 y8 O5 G
  02.3 Fat emulsions maily of type oil-in-water, including mixed and/or flavoured products based on fat emulsions   
, R, L4 P9 D& Q# ]  02.4 Fat-based desserts excluding dairy-based dessert products of food category 01.7  . S1 S5 {- b! O+ M; H7 Q8 \1 C) S
  03.0 Edible ices, including sherbet and sorbet  
( Z5 R& {9 j: B' L  04.1.2 Processed fruit  6 n' E$ B7 g1 z2 n' 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  : x5 X: k% A6 K
  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  
7 K9 V3 v/ B' i' t( r6 s+ a% Y  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  , s3 N8 k7 q1 _4 B- e) G
  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)  
8 o) H/ o3 F& R2 t  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  ) y2 `4 }+ o# P6 ~5 g0 W7 h0 H: q
  04.2.2.8 Cooked or fried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  
- @: L3 N7 {# l* X# t0 ~8 @  05.0 Confectionery  3 o- L8 l; W. y/ D* p. A6 X! a
  06.3 Breakfast cereals, including rolled oats  0 y1 A0 Y4 i4 l+ G" d
  06.4.3 Pre-cooked pastas and noodles and like products  
' ^6 g5 ~8 U# l  06.5 Cereal and starch based desserts (e.g., rice pudding, tapioca pudding)  / t7 v; `! p  u5 \  H6 l' D* \& k8 j
  06.6 Batters (e.g., for breading or batters for fish or poultry)  ) l5 P( D' f! J2 t- I9 J- U
  06.7 Pre-cooked or processed rice products, including rice cakes (Oriental type only)  ( v" M. R/ e8 t
  06.8 Soybean products (excluding soybean products of food category 12.9 and fermented soybean products of food category 12.10)  3 f) m% z' b7 ^
  07.0 Bakery wares  " z8 O5 F' k% w
  08.2 Processed meat, poultry, and game products in whole pieces or cuts  7 f" c5 [; x7 ~* @0 @6 N
  08.3 Processed comminuted meat, poultry, and game products  9 s- k$ S8 t' s
  08.4 Edible casings (e.g., sausage casings)  : S' F# z( z% X$ m7 [
  09.3 Semi-preserved fish and fish products, including mollusks, crustaceans, and echinoderms  
* a& m5 O; s! w$ y  09.4 Fully preserved, including canned or fermented fish and fish products, including mollusks, crustaceans, and echinoderms  ; m; E8 A% `# j+ O- f
  10.2.3 Dried and/or heat coagulated egg products  0 T/ y! a0 g8 t( M3 O. v! a5 g: N. r
  10.3 Preserved eggs, including alkaline, salted, and canned eggs  
, _! b# Z6 R6 |% {7 c0 D  10.4 Egg-based desserts (e.g., custard)  ! q! o% o$ p& {: @0 @
  11.6 Table-top sweeteners, including those containing high-intensity sweeteners  ; [# T( {7 K4 u
  12.2.2 Seasonings and condiments  : W- @! ]' l. J) g
  12.3 Vinegars  
1 h4 m, o) Q  |. ]' ?( Y* ]  12.4 Mustards  1 ]4 I4 K5 A: @1 g+ h3 W
  12.5 Soups and broths  
: Y' i/ b! V8 D& ^  @  12.6 Sauces and like products  
" U1 _/ A: L- h$ s/ \' U, 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  9 ]2 W- g1 e( T5 T4 H3 w3 p" q
  12.8 Yeast and like products  7 j/ C' V" j; C7 N. c
  12.9 Protein products  
: B6 Z4 H/ ^% m, ]/ L5 [  12.10 Fermented soybean products  6 u2 b" D4 g8 E
  13.3 Dietetic foods intended for special medical purposes (excluding products of food category 13.1)  & W/ H2 C, u, x! y
  13.4 Dietetic formulae for slimming purposes and weight reduction  
/ S+ S- G4 w2 [. `3 B  13.5 Dietetic foods (e.g., supplementary foods for dietary use) excluding products of food categories 13.1 - 13.4 and 13.6  
7 y: t; W8 \! R8 X$ q9 m& [  13.6 Food supplements  & ^. ~# v# f8 w% G) f
  14.1.1.2 Table waters and soda waters  
. a4 y1 Z% A0 i/ k4 L& u+ ~4 Y0 q  14.1.4 Water-based flavoured drinks, including "sport," "energy," or "electrolyte" drinks and particulated drinks  
& I3 ]8 {8 }2 ?- D  14.2.1 Beer and malt beverages  ) D) u+ _7 r2 J- ?7 d
  14.2.2 Cider and perry  & C' H, u$ N, {4 y
  14.2.4 Wines (other than grape)  4 v+ d3 q/ ]& [" U0 T
  14.2.5 Mead  & X) r7 a0 K/ D: ?1 x- z
  14.2.6 Distilled spirituous beverages containing more than 15% alcohol  + d# q" @" ~: ?" X! L
  14.2.7 Aromatized alcoholic beverages (e.g., beer, wine and spirituous cooler-type beverages, low alcoholic refreshers)  + m& Y  C, }: M. t, X" T- h
  15.0 Ready-to-eat savouries  
3 k2 O  X# [9 ]/ J  16.0 Composite foods - foods that could not be placed in categories 01 – 15! T5 g$ l0 d( k$ h' ]

& z) R; P- ]1 N
- B6 e( ~) l2 |7 l1 s% Z/ q部分译文:5 T, U& i9 h  s

- `5 O! b( Z2 B* _食品添加剂通用规则
4 B, ]# |" d3 u1 c- w: ^食品添加剂! R; M; V+ O2 o/ U' H9 W3 R
                    二氧化钛(171)
+ P' \, G. X7 z) [1 R3 @食品类别:: l5 J( s: x8 U7 S
06.3 早餐谷类,包括燕麦片
% V2 o' d6 a+ R) y8 y% z) X06.4.3面条及类似产品
4 H( G* G3 x+ ~" c06.5 谷类,淀粉甜点(包括:米粉布丁,木薯布丁)
9 \$ q" C1 b: k- p06.6 面团
. x; J- `! D; J5 U06.7 预煮的或加工的米产品,包括年糕(只包括中式的)06.8 Soybean products : v, A" y( s+ B
07.0 烘焙类
/ ?2 h  T) l, O/ h7 ^6 A$ s07.1 面包,普通烘焙类,以及其混合物
) [* P$ s3 a5 P# C5 Q9 r% `07.1.1 面包,面包卷: o: n+ X8 C' l1 O6 F
07.1.1.1 酵母发酵面包及特殊面包
/ V" B6 X& c/ b9 }+ |" H7 y07.1.1.2 苏打面包
$ x- Z& `; k9 z- h, s4 G* T+ |
' J$ J# [7 w2 O% v8 D6 f2 @0 r% P% Y" q' M" D$ [% Q
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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): f- G  K/ a; J( U5 h

$ t- V+ g" c: m/ F- [: W, T( J! vJECFA关于二氧化钛(钛白粉)的结论0 u/ f2 e) F+ T
3 m* X) X5 B. Q' l  v( t  u
摘要: 2006年JECFA关于二氧化钛的结论
& h- I  i  T: _0 O: D$ U5 FADI值:不作限制。8 D. q3 `1 V6 {7 |$ |  s( f2 |
功能:着色剂5 ~! w3 j4 [+ i; h; {% c+ S
/ a/ j  o' ]: Y) l+ Q/ q
TITANIUM DIOXIDE
' a5 ~  v$ \) J7 [Prepared at the 67th JECFA (2006) and published in FAO JECFA- N( K5 o' v, I, x) d
Monographs 3 (2006), superseding specifications prepared at the 63rd$ Q7 x. M# h0 |0 o; a- b/ d+ @  \) L
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
$ t3 i9 G: O3 NCombined Compendium of Food Additive Specifications, FAO JECFA
, g$ l5 a4 U/ j. JMonographs 1 (2005). An ADI “not limited” was established at the 13th2 z: \; d5 i7 d8 e
JECFA (1969).$ H! h* O% v' P  c
SYNONYMS
6 B" D$ J1 t0 c( WTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171/ z# K  C+ v' J; A2 m5 f; |
DEFINITION8 o7 n0 W- ^% q- a1 B: _
Titanium dioxide is produced by either the sulfate or the chloride2 ^% e+ O3 {* Z( T0 V# v
process. Processing conditions determine the form (anatase or rutile
! p, f( z4 d& Z/ Z& rstructure) of the final product.: [$ K3 c8 |* Z) K3 F
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
4 r& ~: N# d5 Nor ilmenite and titanium slag. After a series of purification steps, the
# j; O, I2 e6 U; x5 @0 A/ tisolated titanium dioxide is finally washed with water, calcined, and; H. D+ ?* I8 u" G7 r1 P
micronized.$ u) S0 H9 j2 c5 n* c9 ~% f
In the chloride process, chlorine gas is reacted with a titaniumcontaining
$ T" `1 S8 m8 c3 Smineral under reducing conditions to form anhydrous1 L/ [/ T, |& r- k% ~
titanium tetrachloride, which is subsequently purified and converted to$ E- `9 I2 W& O
titanium dioxide either by direct thermal oxidation or by reaction with4 |" b/ f6 Y3 B6 \
steam in the vapour phase. Alternatively, concentrated hydrochloric+ p$ t1 l2 G% g' t) b% ]- r9 g+ t
acid can be reacted with the titanium-containing mineral to form a2 o( e; {4 w- O, L
solution of titanium tetrachloride, which is then further purified and
3 v4 D7 J. K2 y2 T9 D. X9 g6 kconverted to titanium dioxide by hydrolysis. The titanium dioxide is
, W! I$ c' G8 `filtered, washed, and calcined.% x' u. ]5 I6 x. Q/ |. Y( C
Commercial titanium dioxide may be coated with small amounts of, F2 N6 j2 R+ q! Y
alumina and/or silica to improve the technological properties of the
6 V  O* q  @0 w( b# Cproduct.
$ ]3 y% N1 ?0 |6 b5 `C.A.S. number 13463-67-7
) `( j% e4 B" }7 vChemical formula TiO2
( X7 C2 \0 F3 k$ l! yFormula weight
3 H, P9 X. X9 h! F4 v+ K/ K79.88: `; l* J0 L+ {. B( U0 L  j; R
Assay
) }0 A1 G. R: y2 L6 ^Not less than 99.0% on the dried basis (on an aluminium oxide and  F$ b2 n. o0 i: l( L
silicon dioxide-free basis)
+ l, f0 B. T1 L' I- B! F7 ZDESCRIPTION$ m9 M! _- J. O- ^5 x) C
White to slightly coloured powder
# ~9 p1 M7 a8 j" p& j% k# |FUNCTIONAL USES
  R0 O# a  A7 u$ e% V. j5 RColour
5 i/ Q& C, P% ^' @$ c' kCHARACTERISTICS
/ w6 P9 w$ c& u% r% h# W  C' oIDENTIFICATION" z$ S' G' ?! ]/ |' s" }7 E, k
Solubility (Vol. 4)) M6 U) A2 i9 R. R8 f
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
2 d" s, {- h' Y/ R7 d2 b- Zsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated, {$ _- B8 i5 y- ^# {  M
sulfuric acid.
" p# x$ s. x: H6 a, u& ~Colour reaction
% m2 l7 |# A6 \: ^% S% FAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
; m0 `% V, o! X% Z/ ]3 vsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with4 }" n4 U8 J2 T: G
water and filter. To 5 ml of this clear filtrate, add a few drops of9 H( G  Q2 {# D6 s: N5 l
hydrogen peroxide; an orange-red colour appears immediately.
( w: K: z( I. m: _/ r# KPURITY
- e$ I4 f* G1 xLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)  h) S& U1 m1 I9 B
Loss on ignition (Vol. 4)" X; X4 s9 p7 Z
Not more than 1.0% (800o) on the dried basis' R5 s$ e2 j( o8 q1 W! V2 ^2 T
Aluminium oxide and/or
0 o3 Q8 X2 G' q# x2 jsilicon dioxide# n+ D2 E8 ?5 m
Not more than 2%, either singly or combined
: `1 ?3 `: O) r! I, H; D7 _: B/ vSee descriptions under TESTS+ X1 u( g. E. J. B; ?
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing, A' I6 j6 k! K2 }
alumina or silica.9 T9 @$ e! E. ^9 p5 Q. a+ Z7 M6 E9 u
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and5 w5 `6 f6 H, E4 D" C
place on a steam bath for 30 min with occasional stirring. Filter: h5 F# r! b- y: P# G9 O! h$ i. i
through a Gooch crucible fitted with a glass fibre filter paper. Wash7 D" F. W% {$ ?9 F
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
( a7 ^- ^9 E7 H- n8 E0 W" X; v9 G0 zcombined filtrate and washings to dryness, and ignite at a dull red
2 |- f  M) H# ~heat to constant weight.1 C7 d* i; i: t4 L. C) M
Water-soluble matter
9 }4 t5 g: c0 V$ H8 \9 W2 ~(Vol. 4)
0 O% F  ~% {: gNot more than 0.5%
/ B' ^& c6 ~- BProceed as directed under acid-soluble substances (above), using2 D) ^2 {9 C- _
water in place of 0.5 N hydrochloric acid.
- t0 _' y0 s! A/ |5 c' X) N% X9 iImpurities soluble in 0.5 N8 z2 g% W  {1 P7 l
hydrochloric acid& }+ K+ y5 |2 ?; Q
Antimony Not more than 2 mg/kg
2 o. `  u. S! mSee description under TESTS
* n) P8 _( B$ AArsenic Not more than 1 mg/kg
3 A; }, A) m  M2 r+ G% wSee description under TESTS
2 z3 C7 N) Q9 o9 \+ K( @Cadmium Not more than 1 mg/kg( T% o/ W) p/ T/ H7 J% _' ^# o/ j
See description under TESTS
- C- A4 Y7 O8 A7 L3 x8 A4 `Lead+ E8 T: Y" \" u  g; W3 D/ E$ f
Not more than 10 mg/kg
& i) u- B& h  Q; B% p8 p( VSee description under TESTS
0 z. P2 J' `: ^$ S5 x+ @/ {Mercury (Vol. 4) Not more than 1 mg/kg
. ?( w) q6 a( d: a; WDetermine using the cold vapour atomic absorption technique. Select a
1 u. m9 N* o+ w6 K8 e, Fsample size appropriate to the specified level
* M. e6 [& g% C9 i, M3 a2 QTESTS. f1 Q, u1 F7 ?
PURITY TESTS
0 j) N4 m2 _  b& B% n7 [7 l2 V  }) nImpurities soluble in 0.5 N
6 M6 l  u3 o! f0 @/ ~8 l+ {hydrochloric acid
1 V  ^8 S8 N8 S$ B' `6 lAntimony, arsenic,
4 @6 A/ c2 Y+ E/ V5 zcadmium and lead6 H3 x) U" b! A5 `( k
(Vol.4)' A' z$ i! T! A. ?) |: |
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N2 n" D& ~9 }- Q( p' G
hydrochloric acid, cover with a watch glass, and heat to boiling on a
7 ?: ~, B) o  W/ Q- A! q# w  zhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml7 @& y8 Z6 J# X$ m8 e5 y! N7 I( i
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved& s# T7 c: @- @8 R" U1 {
material settles. Decant the supernatant extract through a Whatman: |7 u: e2 r9 Y+ {0 b% j+ \6 G
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml; o* E  W- Z. @1 Y, C9 [
volumetric flask and retaining as much as possible of the undissolved  ~" ?9 f" M$ B% j
material in the centrifuge bottle. Add 10 ml of hot water to the original
% E3 p4 {$ b! Y& Kbeaker, washing off the watch glass with the water, and pour the
' A: ~7 G% q% y, L4 qcontents into the centrifuge bottle. Form a slurry, using a glass stirring0 w5 T/ a1 R6 r# I1 D4 C
rod, and centrifuge. Decant through the same filter paper, and collect$ z; e* T, E# ^9 H
the washings in the volumetric flask containing the initial extract., Q+ l9 x( X. y, x& }9 e
Repeat the entire washing process two more times. Finally, wash the
  j7 ?5 Y" U0 ?0 g8 h$ R- l$ mfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
5 P' I  y3 w3 b8 ^- f: {to room temperature, dilute to volume with water, and mix.
5 r( P$ S' W0 T6 ?  Z$ c, wDetermine antimony, cadmium, and lead using an AAS/ICP-AES
. i' ]9 O. N) ]/ f" utechnique appropriate to the specified level. Determine arsenic using the
/ P0 r$ D; q+ Y/ z& X4 [7 F. EICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
0 O+ P5 K1 o/ @) J2 ]Method II of the Arsenic Limit Test, taking 3 g of the sample rather than! t9 z, _) Q0 r# |0 `, T5 S8 z$ r
1 g. The selection of sample size and method of sample preparation
5 B  O! \1 y8 ?3 \' o  Mmay be based on the principles of the methods described in Volume 4.6 M( a% @; B, i
Aluminium oxide Reagents and sample solutions
( k# b) O/ q. s0.01 N Zinc Sulfate5 O! {, j% f! ]; c
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to' m# y$ k8 u; U- G3 ~3 p, l
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
! Q, E; J3 E! l" U% t% h' Mof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of' }. l' D& u3 u' E% G
concentrated hydrochloric acid, heating gently to effect solution, then/ u) c, C8 ]0 Y. Y- Q
transfer the solution into a 1000-ml volumetric flask, dilute to volume3 C1 Y, K1 a. u
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5000 ~0 d9 v1 l* h3 ^$ C; n8 |
ml Erlenmeyer flask containing 90 ml of water and 3 ml of/ M0 l$ e( x3 ?
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
8 H" A' T0 d8 G. N1 }; h/ M25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
% H8 t& ?2 t$ w) @( @dropwise, ammonia solution (1 in 5) until the colour is just completely. j$ i' e0 o6 Y( W, \* H
changed from red to orange-yellow. Then, add:
7 `3 z( D2 T  H(a): 10 ml of ammonium acetate buffer solution (77 g of
; A! V- e" b9 R- Tammonium acetate plus 10 ml of glacial acetic acid, dilute to+ V" `, q3 W4 Q- H5 F; A& ]
1000 ml with water) and& B  p8 n% ^) Y7 L( D3 O
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
4 v, d  D# [% G3 j( cof diammonium hydrogen phosphate in 700 ml of water,
' D% ~: l; ^0 g4 C: c% g% }( badjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
# ]3 O+ H2 T$ Uthen dilute to 1000 ml with water).* S3 k( ]4 O3 ]( U) W
Boil the solution for 5 min, cool it quickly to room temperature in a  r" S. \: ^( D& T/ C2 P
stream of running water, add 3 drops of xylenol orange TS, and mix.
2 K3 c2 g) b& TUsing the zinc sulfate solution as titrant, titrate the solution to the first; x/ P  n3 L5 E
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
& O) V) Z- C; H, j* }This titration should be performed quickly near the end-point by9 \0 `# Y8 f/ j( m, w. h/ @
adding rapidly 0.2 ml increments of the titrant until the first colour% A/ {3 z# J$ ^! j3 N
change occurs; although the colour will fade in 5-10 sec, it is the true
4 r) p% E" U- ?0 J: kend-point. Failure to observe the first colour change will result in an
  \1 r& P2 B8 N4 Aincorrect titration. The fading end-point does not occur at the second
/ _& e3 H7 @) G, j6 [% cend-point.)4 X) F$ d: \6 W; T, W$ l
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a3 g' V. n: t3 E5 l7 f3 t  I5 {
stream of running water. Titrate this solution, using the zinc sulfate( N$ ]( ~8 \; x/ ^
solution as titrant, to the same fugitive yellow-brown or pink end-point
' B$ q# }! ]+ }' o6 N6 e6 ~as described above.
" W% ]! `. {$ o3 v+ F- f; z* bCalculate the titre T of zinc sulfate solution by the formula:% t9 k: ^& W+ N
T = 18.896 W / V9 P1 k. w+ Q$ C! r3 g+ F  ]) X/ T
where9 v6 _+ h8 p& C0 l7 }6 R( M
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution$ ?9 Q  `( z2 e  u  i0 |2 P' n. D
W is the mass (g) of aluminium wire
- k6 n0 @9 v' p- d& v4 g& JV is the ml of the zinc sulfate solution consumed in the
. P  _: N4 h4 E& `8 ssecond titration  R2 H2 G3 a4 E; `% L5 u
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
/ `/ r7 Z% p8 G( A' CR is the ratio of the formula weight of aluminium oxide to
* ^8 H' j0 m) s8 G. m  ?that of elemental aluminium.
( {0 H0 y2 ?8 _! j8 d( sSample Solution A
2 R  J8 Y7 k- ?4 Y+ f2 T, vAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
- }2 A) y; `: H3 x( p/ zglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).4 o9 a- ~# w6 c2 Y" M
(Note: Do not use more sodium bisulfate than specified, as an excess& Y& O# q8 z, [3 c
concentration of salt will interfere with the EDTA titration later on in the. i# O( O: r7 E0 {0 f1 Y
procedure.) Begin heating the flask at low heat on a hot plate, and# e; ?8 m: N0 j0 w: X
then gradually raise the temperature until full heat is reached.7 _7 k; l/ `* m, [* y9 v% O" S
(Caution: perform this procedure in a well ventilated area. ) When! j& Q6 z$ W3 Y
spattering has stopped and light fumes of SO3 appear, heat in the full6 C, M* y0 Z+ H( P9 O% S" K* M6 p
flame of a Meeker burner, with the flask tilted so that the fusion of the: n3 \& v6 R) F3 [1 m& b6 a( ?' a
sample and sodium bisulfate is concentrated at one end of the flask.
! y! e3 H  T& `) p( @: P0 [) NSwirl constantly until the melt is clear (except for silica content), but
; n4 q/ a! v9 G9 {' B  Q+ z" o) ?guard against prolonged heating to avoid precipitation of titanium" w' D. Y( N* X  W
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until0 g- @6 z" \2 T
the mass has dissolved and a clear solution results. Cool, and dilute to: j, |/ M4 P$ Y( e( F
120 ml with water. Introduce a magnetic stir bar into the flask.
9 S+ G, y) N5 XSample Solution B
4 q0 T, b, L/ S" ~9 a: V' ~Prepare 200 ml of an approximately 6.25 M solution of sodium
" h; c- _; z; q* I! Chydroxide. Add 65 ml of this solution to Sample Solution A, while5 z0 s% M; r) b) e
stirring with the magnetic stirrer; pour the remaining 135 ml of the7 j6 n9 U5 B7 e
alkali solution into a 500-ml volumetric flask.( p4 ]7 E) t+ r! D$ `
Slowly, with constant stirring, add the sample mixture to the alkali
) n, P9 R8 l2 rsolution in the 500-ml volumetric flask; dilute to volume with water,
0 ~/ f6 _3 e% i) b+ D  H- L* r6 gand mix. (Note: If the procedure is delayed at this point for more than
1 a- n' [9 e' Y2 hours, store the contents of the volumetric flask in a polyethylene* B4 b3 C/ [" `8 k4 [/ B; T
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
% K7 j, [$ t8 b2 i7 B$ {" J) s, y6 d! Vthen filter the supernatant liquid through a very fine filter paper. Label7 L6 k, b7 \, p' s
the filtrate Sample Solution B.8 I$ x4 Y: |- q3 k5 S# E; i
Sample Solution C' m1 O$ Q* u7 w
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
5 v1 s3 X1 L( i* B2 I, k- r$ l  Rflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid  f$ T0 Y9 ?5 |/ H* E; M6 R3 q/ `
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
+ Q8 j: \2 I6 T6 w5 o; jM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is- }, T$ s5 `: N8 ~4 u3 ]
known, calculate the optimum volume of EDTA solution to be added  F% E7 \% s1 m+ C# h: ?
by the formula: (4 x % Al2O3) + 5.]& x3 Z4 I0 M3 ^, ]2 C
Add, dropwise, ammonia solution (1 in 5) until the colour is just
, T% L, u% j" U3 ocompletely changed from red to orange-yellow. Then add10 ml each
( ^% X, y) X6 j" p7 t" b9 T3 g% qof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
: J0 w  o. C1 m, T7 W( a( c6 Froom temperature in a stream of running water, add 3 drops of xylenol5 |# K" v9 L; p, j1 f1 m4 _
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
& _3 z0 [/ z& k% s4 |bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
6 m7 y5 i* w. c; ?' y8 x: r- SpH, a pink colour indicates that not enough of the EDTA solution has; U% v8 T* O0 W8 k. |
been added, in which case, discard the solution and repeat this& G, Z! ]0 p* ]" a7 A, ?  [) u; P
procedure with another 100 ml of Sample Solution B, using 50 ml,9 {. E3 F4 E& i5 d
rather than 25 ml, of 0.02 M disodium EDTA.
; ?1 g3 R$ }# xProcedure
" i, ?+ p, ~/ Y3 Z% |- i& T) X2 ^Using the standardized zinc sulfate solution as titrant, titrate Sample
$ a$ ]1 p5 h3 kSolution C to the first yellow-brown or pink end-point that persists for
- `/ Q  e7 \: n3 w$ _1 f5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first6 e4 J3 e& b$ K! e% d
titration should require more than 8 ml of titrant, but for more accurate5 r4 @/ Q$ J3 S
work a titration of 10-15 ml is desirable." T# \* b+ P: {5 P, o  p! n  y
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-50 M% v# z& |* ?
min, and cool in a stream of running water. Titrate this solution, using
0 M4 _7 N& C8 n6 k% x# Fthe standardized zinc sulfate solution as titrant, to the same fugitive% P* l& [2 K0 \- S8 H
yellow-brown or pink end-point as described above.
2 o# R2 B7 {/ }& f' `5 r) k1 xCalculation:8 F# h  X* z. k) Q. F% ?: @, y
Calculate the percentage of aluminium oxide (Al2O3) in the sample
5 X1 c( U  n5 q; _3 Btaken by the formula:8 a: U) n5 _& c9 d; L' y( ^- a
% Al2O3 = 100 × (0.005VT)/S. W7 N; X1 p5 g2 d7 h
where
- g. ]7 C& o( u9 JV is the number of ml of 0.01 N zinc sulfate consumed in
# Z6 g) t! Z/ x5 Pthe second titration,1 d) q; l6 B; ~: b! d7 A4 n# {& N
T is the titre of the zinc sulfate solution,
) l: q+ k' l2 f; Z0 V5 O* MS is the mass (g) of the sample taken, and
' a0 n7 o. e5 ]- f6 x0.005 = 500 ml / (1000mg/g × 100 ml).+ S8 [" r# I& J- E2 a/ e# u3 a( j
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica5 O- t4 z  G3 G$ N
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
4 s; l& N7 g4 v; G7 }$ I2 r( j6 AHeat gently over a Meeker burner, while swirling the flask, until
2 K$ q( O0 S3 n6 `" X1 k- Cdecomposition and fusion are complete and the melt is clear, except2 W/ k( _- X; Y5 A4 L% ?% X+ _
for the silica content, and then cool. (Caution: Do not overheat the; v' {- l' U5 o" d
contents of the flask at the beginning, and heat cautiously during: O8 ^. o& m4 {% m, |5 g) Z$ d
fusion to avoid spattering.)- J$ U5 |6 ~2 L% C& h  h
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
9 x) n, W- B, dcarefully and slowly until the melt is dissolved. Cool, and carefully add' F; A2 A2 w' R2 M( \* N. P
150 ml of water by pouring very small portions down the sides of the
* k" }1 n9 s+ ]6 p' V9 n0 Dflask, with frequent swirling to avoid over-heating and spattering. Allow
3 r, ^# \, ^$ L# K" k+ p2 rthe contents of the flask to cool, and filter through fine ashless filter5 a2 x. j# \: {! z5 V- n, m
paper, using a 60 degree gravity funnel. Rinse out all the silica from
; m; B( [$ j. s; S7 Z0 _the flask onto the filter paper with sulfuric acid solution (1 in 10).$ n9 ]3 _. Y6 |& y; r
Transfer the filter paper and its contents into a platinum crucible, dry in/ ~: _) [0 w* b: C2 v6 ~6 U+ f
an oven at 1200, and heat the partly covered crucible over a Bunsen
1 k8 y( L5 J1 f" u2 p& tburner. To prevent flaming of the filter paper, first heat the cover from
/ T/ J- q5 X0 babove, and then the crucible from below.
* i- D! X2 U- S; T" J8 B" z) fWhen the filter paper is consumed, transfer the crucible to a muffle# Q2 r  s% Q* i! C
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
, g. s7 ?- S3 Jweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
9 ]2 m7 p3 C8 M( h( o. m1 {  {hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first1 ?$ X% y/ L0 u% U: Z& W1 h! k
on a low-heat hot plate (to remove the HF) and then over a Bunsen: N5 S. \, @* w- s/ J8 J& ?
burner (to remove the H2SO4). Take precautions to avoid spattering,
  M% E5 r9 V3 g7 e# }# Q, |4 R# Lespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
3 u# h1 t  h# T# k* l. I, edesiccator, and weigh again. Record the difference between the two# u& [- W3 y  P
weights as the content of SiO2 in the sample.
  z/ i! b! u1 v5 W- iMETHOD OF ASSAY
4 _+ P* d" @7 T6 X2 ~9 n# QAccurately weigh about 150 mg of the sample, previously dried at 105o
9 a2 H+ [! W% I4 Z, ~( V- Z/ Ufor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water  o0 z& \( `2 c6 M1 F9 w. V5 o
and shake until a homogeneous, milky suspension is obtained. Add 30
4 t5 }+ j! w. Uml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially! w* @! y2 E' T9 |9 W
heat gently, then heat strongly until a clear solution is obtained. Cool,
! Q' \% S3 B7 j8 X9 Kthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric; y) E% ]# y! E+ \3 M
acid, and stir. Add 3 g of aluminium metal, and immediately insert a( l1 o* L0 L8 E6 Z" T
rubber stopper fitted with a U-shaped glass tube while immersing the% o! Y$ j& Y3 J2 l( E+ S6 ^( _  C0 W" |  |
other end of the U-tube into a saturated solution of sodium/ s$ U  I0 g, w( Q6 B
bicarbonate contained in a 500-ml wide-mouth bottle, and generate# |7 u* n/ Q, u
hydrogen. Allow to stand for a few minutes after the aluminium metal" d- X. Z1 }& B7 K: X4 m/ l
has dissolved completely to produce a transparent purple solution.% }+ \7 @) a7 n6 D$ y: P
Cool to below 50o in running water, and remove the rubber stopper+ @6 o% s& A3 w& s7 l) P
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
! c( p6 p- ]* O1 n, a' W2 Msolution as an indicator, and immediately titrate with 0.2 N ferric# H1 j; y9 |% C: [
ammonium sulfate until a faint brown colour that persists for 30
* ]* ]$ z+ `, Y/ |3 tseconds is obtained. Perform a blank determination and make any
" v. c, g# O! j2 G/ B# n1 G6 Tnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is0 y2 e# i( ^5 P* O
equivalent to 7.990 mg of TiO2./ p* M* C$ C4 M2 G
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