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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) % f5 e4 ]1 s  f& {& L. y% T8 ^( v0 y& H

( N  Y6 s, l% S, Y9 h3 |* j( B- f0 g
. l7 H5 v8 N% C& l; |6 K$ OCAC关于二氧化钛(钛白粉)的使用规定2 a1 w' Z, A$ F' p; Z- b7 [
GSFA Online " D  z9 u1 C# |3 d, E" D9 G5 g
Food Additive Details
2 w& P) I" @2 G0 P6 D  l( U1 rTitanium Dioxide (171)  {5 ?* |1 j2 w3 C, o6 m- i! {" ?
Number Food Category  
1 n& w4 r- j0 ]1 d, G# ~1 W9 D  01.1.2 Dairy-based drinks, flavoured and/or fermented (e.g., chocolate milk, cocoa, eggnog, drinking yoghurt, whey-based drinks)  , [! y$ m* n. \+ {4 D% f
  01.3 Condensed milk and analogues (plain)  
5 W; P0 S9 U3 {2 y. s+ [& H4 w  V  01.4.3 Clotted cream (plain)  ! e* \% }* z) w) l
  01.4.4 Cream analogues  6 Y3 N. F( s$ c+ d$ @) y$ Q! L
  01.5 Milk powder and cream powder and powder analogues (plain)  
& A. c- K4 ?. H  01.6 Cheese and analogues  * A- ]8 s) r) M
  01.7 Dairy-based desserts (e.g., pudding, fruit or flavoured yoghurt)  
9 D: d# S7 `8 q9 u2 }( m. ]  01.8 Whey and whey products, excluding whey cheeses  ) B' G* g9 q% Z7 t- |" s  C& E
  02.2.1.2 Margarine and similar products   " L2 _" W# ]5 }! D
  02.2.1.3 Blends of butter and margarine  
2 t! U: Y. y0 m  02.2.2 Emulsions containing less than 80% fat   
# l6 r7 B" {! c4 q  02.3 Fat emulsions maily of type oil-in-water, including mixed and/or flavoured products based on fat emulsions   
' B, P+ M7 Y" n  02.4 Fat-based desserts excluding dairy-based dessert products of food category 01.7  
2 r$ X' S# A" |9 E9 A  03.0 Edible ices, including sherbet and sorbet  
5 y, l$ _6 a2 V- E! {5 _  04.1.2 Processed fruit  : @0 [1 m$ O6 k& O7 R
  04.2.2.2 Dried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweeds, and nuts and seeds  ) ]4 I' A) J7 A# j2 T% d' [: }5 e
  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 M! f* B* R8 I- K. ~' 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  
2 \# J; M! G; \- R0 C. R7 v; H3 K  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)  
: B; `" o" z( E0 l- R: N" o  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  
+ `$ s$ e% \% @  04.2.2.8 Cooked or fried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  & b0 w+ R; E6 A: D! Z+ X0 O5 G
  05.0 Confectionery  
. A( Q% \# ~+ y9 R  I  06.3 Breakfast cereals, including rolled oats  
! `) ~9 h5 ?$ V  06.4.3 Pre-cooked pastas and noodles and like products  
+ ]) I' o  H) w  06.5 Cereal and starch based desserts (e.g., rice pudding, tapioca pudding)  
3 W  n& |, A0 x! e  06.6 Batters (e.g., for breading or batters for fish or poultry)  
; c9 G& D4 X4 i. \1 {: Z2 e0 U  06.7 Pre-cooked or processed rice products, including rice cakes (Oriental type only)  
8 e2 k3 h# I$ j$ o9 B* ?  06.8 Soybean products (excluding soybean products of food category 12.9 and fermented soybean products of food category 12.10)  
( J( N. P! G' ^+ Q  T' E  07.0 Bakery wares  
7 F9 M, J# `6 O) R  08.2 Processed meat, poultry, and game products in whole pieces or cuts  & i7 O+ J' K' ^
  08.3 Processed comminuted meat, poultry, and game products  2 @6 P1 i+ I: v! ^1 v7 M, c
  08.4 Edible casings (e.g., sausage casings)  
- f7 t  V8 K. w- Y$ ~' W! }- Z0 q  09.3 Semi-preserved fish and fish products, including mollusks, crustaceans, and echinoderms  % ^/ r. M* i/ k* R+ @
  09.4 Fully preserved, including canned or fermented fish and fish products, including mollusks, crustaceans, and echinoderms  
" y- T; a$ ?$ z; e! |, c  10.2.3 Dried and/or heat coagulated egg products  
6 T1 t+ j0 D0 x& w  10.3 Preserved eggs, including alkaline, salted, and canned eggs  
* {, H2 i  V5 L( Z) U  10.4 Egg-based desserts (e.g., custard)  
, r; u- p, u5 x  11.6 Table-top sweeteners, including those containing high-intensity sweeteners  + X' h4 I1 f4 E& s; X" s! C
  12.2.2 Seasonings and condiments  5 s% w1 {0 ?2 t8 P
  12.3 Vinegars  7 b3 W' o/ E& F2 F" \
  12.4 Mustards  # A8 n: K9 y- k
  12.5 Soups and broths  : e! }% W$ m) e7 K; G6 i- X
  12.6 Sauces and like products  
4 r1 x* c9 C9 y1 |' m7 R8 u  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  
7 o2 A1 C! O5 U; j  12.8 Yeast and like products  2 X3 s  n) X) C0 g. A
  12.9 Protein products  
+ {$ J5 y& v; B/ \  12.10 Fermented soybean products  1 l' _. E  Q! h$ c6 u+ d( ~
  13.3 Dietetic foods intended for special medical purposes (excluding products of food category 13.1)  % o5 R& p) A( {% T
  13.4 Dietetic formulae for slimming purposes and weight reduction  
! i# L: I4 S  \6 ~* v" x# @( }  13.5 Dietetic foods (e.g., supplementary foods for dietary use) excluding products of food categories 13.1 - 13.4 and 13.6  
7 E2 }" \* Z: N' t/ H  13.6 Food supplements  
" I+ Z7 J! z! s9 d  14.1.1.2 Table waters and soda waters  3 o& w/ g" B% g2 |2 s
  14.1.4 Water-based flavoured drinks, including "sport," "energy," or "electrolyte" drinks and particulated drinks  
3 \& d7 w5 V! V- q1 l  14.2.1 Beer and malt beverages  " @7 L8 B- @$ Z) Q
  14.2.2 Cider and perry  3 K( L6 ]9 X# S$ ?) h( d
  14.2.4 Wines (other than grape)  4 r/ @3 T+ c- x+ m# |
  14.2.5 Mead  3 g  M+ E: Q4 j8 s
  14.2.6 Distilled spirituous beverages containing more than 15% alcohol  - O4 M4 X) ^5 R% O4 H4 F
  14.2.7 Aromatized alcoholic beverages (e.g., beer, wine and spirituous cooler-type beverages, low alcoholic refreshers)  9 J/ [9 _3 M# L$ W% C0 k  ^
  15.0 Ready-to-eat savouries  , p  Q2 J' x1 [+ R/ x5 I5 x' t
  16.0 Composite foods - foods that could not be placed in categories 01 – 154 `! }! L9 u0 [* s* g6 B# L
& j. u/ ?$ [0 e: `0 y) S6 l6 W# X; s% I( {

! M* A$ s* e0 Z' Q/ I$ L部分译文:
$ d9 P1 s/ ?. b" C. G  |; X! i* ^& x$ u1 e3 J3 i
食品添加剂通用规则
& M5 M% M! M& Z食品添加剂
- A. u. A% T% a+ @$ X* y! \                    二氧化钛(171)
6 s2 n. o, @; m食品类别:
  o: }6 `# q# s/ h: K0 C& E/ D- a06.3 早餐谷类,包括燕麦片
+ j* X- B0 @) T1 V: ~4 I' p* m06.4.3面条及类似产品" d* c( \- c( p6 O% \
06.5 谷类,淀粉甜点(包括:米粉布丁,木薯布丁)1 X4 {3 v4 W3 R* C
06.6 面团
6 {  P) ^+ E- v" Q, _5 }8 X06.7 预煮的或加工的米产品,包括年糕(只包括中式的)06.8 Soybean products ; B: c* A* D( Y* R. P( D- ]
07.0 烘焙类
" ]6 ?9 L/ O9 K- s07.1 面包,普通烘焙类,以及其混合物: M7 t; @; b% D/ ?
07.1.1 面包,面包卷# m+ O3 p" A% h  J+ ^+ d& z
07.1.1.1 酵母发酵面包及特殊面包
; J1 c8 j( f+ I) i; x07.1.1.2 苏打面包7 L. a+ ^) o  w
( @6 ~7 A! c% O. N& M
4 F1 j) _; R8 v( o' T9 L2 G
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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)
  V7 \8 P' M8 T$ [2 C( u
! H  i6 X' d, m& A  Q/ E7 G( J  t% j# FJECFA关于二氧化钛(钛白粉)的结论; s2 I, ?1 z- d) L  E; |

1 |8 I' p, h. V1 m3 i摘要: 2006年JECFA关于二氧化钛的结论6 o- y7 f7 M" B5 Z$ n' P; A) I
ADI值:不作限制。9 q! J4 K; f% R; s* G
功能:着色剂
& w6 {* R! }3 v1 p5 w* \8 W; Y& J/ c
TITANIUM DIOXIDE
. x1 w2 _1 A$ J# W9 I7 tPrepared at the 67th JECFA (2006) and published in FAO JECFA
- z" g8 ]3 `% e5 MMonographs 3 (2006), superseding specifications prepared at the 63rd
7 `, \; o0 g2 L8 ]( NJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
7 G; e/ m. H2 Y: O- t5 dCombined Compendium of Food Additive Specifications, FAO JECFA
2 b; _0 N" n; W# s; D) NMonographs 1 (2005). An ADI “not limited” was established at the 13th- v7 ~7 k& s1 N1 y, u1 b
JECFA (1969).
  C" n; O3 F0 s. D8 h3 XSYNONYMS5 |; J" o+ c' R- T* Q
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
* r3 |- N4 z. C/ V; V+ WDEFINITION. U- |4 ?9 a2 O+ S, z5 G
Titanium dioxide is produced by either the sulfate or the chloride
. F# h* _5 |- A( V+ |9 ~% d: oprocess. Processing conditions determine the form (anatase or rutile
7 _! b3 X$ o( c0 Ustructure) of the final product.
& y; \, |8 ~6 S6 r, @1 S% XIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
5 q2 q+ u3 M" kor ilmenite and titanium slag. After a series of purification steps, the8 O4 U5 E2 n$ k$ I
isolated titanium dioxide is finally washed with water, calcined, and+ A8 ~4 S+ U* @: X" s
micronized.4 o# O# T( |& A3 N* \
In the chloride process, chlorine gas is reacted with a titaniumcontaining
* I5 E) a; _/ `5 Y& ^6 q) G- Gmineral under reducing conditions to form anhydrous" g! l5 Z( o. V. ^
titanium tetrachloride, which is subsequently purified and converted to; C8 ?% ~1 Y1 ~* D! Q* w, O' A1 I
titanium dioxide either by direct thermal oxidation or by reaction with
( }! j# Z( J( v4 y( @steam in the vapour phase. Alternatively, concentrated hydrochloric
+ l: K) m" g7 T. O+ macid can be reacted with the titanium-containing mineral to form a
: v6 F/ X2 O7 K  Q7 qsolution of titanium tetrachloride, which is then further purified and
& J; p8 o9 B0 {* N4 D7 R3 i3 L7 Qconverted to titanium dioxide by hydrolysis. The titanium dioxide is
, W5 x$ p5 Q2 g% t& r+ R) Ofiltered, washed, and calcined.
0 V7 Z+ K6 `+ q8 m; \Commercial titanium dioxide may be coated with small amounts of
) p0 W, ~7 c9 M- |/ Ualumina and/or silica to improve the technological properties of the1 ]5 X7 V+ o  o# W+ _# T( l7 D
product.) u- V8 v: V9 g+ z. V" \
C.A.S. number 13463-67-7) q  k2 Q. i/ b4 \$ ?& J
Chemical formula TiO2- g4 n# ?3 I% C# k
Formula weight+ W- K5 o) T" O! v5 G0 S
79.88
6 A7 k6 t5 i+ N* n) H7 T" j8 V: LAssay
; J* @7 C6 c3 DNot less than 99.0% on the dried basis (on an aluminium oxide and
5 p/ T- v" C! F6 ]4 |$ ^- C3 Tsilicon dioxide-free basis)( p2 {8 Z6 v0 w- Q, `
DESCRIPTION& ?6 ^: h2 J+ H5 w
White to slightly coloured powder
* R' \$ l& j4 N, E" B9 YFUNCTIONAL USES
. O6 X) O) k, Q% K0 E- WColour
6 p, K" z/ k9 y. Y% A3 \4 D6 dCHARACTERISTICS
, |  o8 w) p% P) b, TIDENTIFICATION
/ }$ p3 n# g) Q6 t4 gSolubility (Vol. 4)
2 F% m& {  Y% }7 }# [' R/ F# W$ ZInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
0 ?/ Z# V0 c# V: Y3 p) J. G+ |! B) {solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
" e4 l' @: M) ssulfuric acid.$ Z: x8 ^0 y+ b, q
Colour reaction8 }5 ~# C8 s8 I7 W  E. M
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
5 \0 E. a% n+ isulfuric acid appear, then cool. Cautiously dilute to about 100 ml with5 _4 b- J& \, U/ W# }; h/ v
water and filter. To 5 ml of this clear filtrate, add a few drops of
0 n* v7 l% t0 K$ j. }! mhydrogen peroxide; an orange-red colour appears immediately.0 _' M0 C. @$ @$ b8 Y- {: B
PURITY
) W3 F" ^$ q! vLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)4 l* ?" e  {0 _5 j4 z  ~0 {1 `2 b* t
Loss on ignition (Vol. 4)
  h9 l) I* Y" a% u/ `' H9 |6 KNot more than 1.0% (800o) on the dried basis
( \" e7 s* g. ~' wAluminium oxide and/or4 Q' ~- {" A8 z* Y7 G
silicon dioxide$ U2 b' G' s- d% w0 d
Not more than 2%, either singly or combined+ F, D! ]/ X6 i- z) ?! N8 ?$ H
See descriptions under TESTS+ D* a7 ]/ ?- ]7 {0 [
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
$ c" @: c1 Y9 V7 Y. b7 Falumina or silica.& }* O( w) n! w% r
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and0 B) O4 c+ A8 N1 m) D
place on a steam bath for 30 min with occasional stirring. Filter' w  a8 P9 J2 L$ u
through a Gooch crucible fitted with a glass fibre filter paper. Wash" r7 b6 R" Z' ~3 o
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the8 R) H) W  S  `2 y6 X' L
combined filtrate and washings to dryness, and ignite at a dull red
: K& t+ g: d/ l; y" Z8 ?( V, oheat to constant weight.
/ P) i& U/ A4 R5 zWater-soluble matter
* R' u2 r7 d# c! a(Vol. 4)) t5 {. u  \# h0 [/ I' v& o
Not more than 0.5%* b- E4 v& g; f$ N- g* o
Proceed as directed under acid-soluble substances (above), using
+ i" o1 S) C% a: |! W* ~$ Mwater in place of 0.5 N hydrochloric acid.
- A" J( `6 e2 E' J3 m, tImpurities soluble in 0.5 N( y, |$ ]- w/ K! w) d, _
hydrochloric acid
* o  ~) F9 {* {- y! rAntimony Not more than 2 mg/kg# d7 _, M7 D2 J  X
See description under TESTS4 M3 n" Y2 a3 W+ ~! _7 p* h. I6 y
Arsenic Not more than 1 mg/kg
6 P& R) x3 A* Q: l. d! ~( K* J- rSee description under TESTS$ n" f* f, b+ S: a& t) U1 {) V0 ~
Cadmium Not more than 1 mg/kg
0 `- L! \0 f) K' kSee description under TESTS; N/ R' p4 n9 j: j# ?% J
Lead
/ X+ o* l3 E( X+ @: F5 cNot more than 10 mg/kg: y+ w: _/ h9 W9 J( @
See description under TESTS
/ D) [# R0 N5 M0 PMercury (Vol. 4) Not more than 1 mg/kg
8 n% ~+ S* Z. d2 RDetermine using the cold vapour atomic absorption technique. Select a+ P" ]% B) i. G3 ^6 H
sample size appropriate to the specified level% l! K, d3 u, O6 @/ ^- C' \; u* D
TESTS3 d7 ]% n5 n$ f, |% n# D- Y
PURITY TESTS
- p7 _6 y3 G' ^* v+ t0 b+ qImpurities soluble in 0.5 N% E/ B( [. [0 Y8 G8 h! z' k5 ?
hydrochloric acid$ U0 C* _* b5 C0 s
Antimony, arsenic,, K# C1 M7 m; Q) K  J
cadmium and lead
- o) T$ B: Z# x+ E& y' h(Vol.4)$ |" \* T5 d' z
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
4 Y2 H6 j! z5 V( \8 O0 q  ~& nhydrochloric acid, cover with a watch glass, and heat to boiling on a# W% I0 t  O' H  R7 f
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
+ W1 \7 }1 M6 l% k1 ]5 z2 K  Rcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
) d+ S+ [, E, q- C1 X+ k' l( x* Umaterial settles. Decant the supernatant extract through a Whatman
- F# ^0 e, v/ ]& c1 NNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml; x8 R# o! X5 P! Z3 j! x
volumetric flask and retaining as much as possible of the undissolved
7 L" t0 I& D! F/ Tmaterial in the centrifuge bottle. Add 10 ml of hot water to the original5 n5 c6 G; ^4 m. Q# c6 g  t! c
beaker, washing off the watch glass with the water, and pour the
6 I$ G1 m0 g) v0 c! gcontents into the centrifuge bottle. Form a slurry, using a glass stirring
# c! n& Y6 X4 @3 k$ G8 crod, and centrifuge. Decant through the same filter paper, and collect
# `( Y' F1 L1 Athe washings in the volumetric flask containing the initial extract.
2 O/ S6 q1 J4 H( }/ NRepeat the entire washing process two more times. Finally, wash the3 k4 w, E/ w8 R5 n& c
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask* N( ~, D: ^; m6 C
to room temperature, dilute to volume with water, and mix.
6 D% y! R6 J  yDetermine antimony, cadmium, and lead using an AAS/ICP-AES' E+ `. e' H9 {; T9 a
technique appropriate to the specified level. Determine arsenic using the
: a. M! w  a) b/ f" G$ T  J" VICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
3 O% k6 b; y* L: _Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
9 V- s3 a9 ~  {$ n; O/ p8 t* w1 g. The selection of sample size and method of sample preparation
  i0 p( {8 n  u0 C$ I+ u( h0 amay be based on the principles of the methods described in Volume 4.4 c/ u+ {! u& I6 d. J) W3 a; P
Aluminium oxide Reagents and sample solutions* E" d0 k: x/ j9 |, A) b
0.01 N Zinc Sulfate9 S* ^9 e. r+ t* O6 ]" T" j
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
. V- f- F' V& D2 ^make 1000 ml. Standardize the solution as follows: Dissolve 500 mg8 T3 y- i% I" C, ~* F3 U5 t9 f2 k
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of0 g9 x4 K# e# n8 a
concentrated hydrochloric acid, heating gently to effect solution, then
0 l" w, B+ L7 b7 G# M4 Y, Q8 _transfer the solution into a 1000-ml volumetric flask, dilute to volume
& @4 Z; j; a4 S6 kwith water, and mix. Transfer a 10 ml aliquot of this solution into a 5000 I2 x. m2 U% d- N3 r$ j
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
" c( M6 S  Y# A) T* N7 m* Kconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
  F: y& p$ y+ H8 L2 s25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,$ v- C/ q8 ?, e- n0 D5 v# R
dropwise, ammonia solution (1 in 5) until the colour is just completely5 e, |6 C4 l# H7 c9 P3 Q. Z1 ~0 S
changed from red to orange-yellow. Then, add:) D" m' O$ a4 E
(a): 10 ml of ammonium acetate buffer solution (77 g of
9 L- N1 T5 Q" c& _. e: H# b6 Rammonium acetate plus 10 ml of glacial acetic acid, dilute to
1 y9 E9 @1 l: Y! @1000 ml with water) and
! E. ~$ J& l' ]6 j6 V; x) ](b): 10 ml of diammonium hydrogen phosphate solution (150 g
* c) K. w9 e. {* w+ C, e' A7 t: Rof diammonium hydrogen phosphate in 700 ml of water,. Y, s9 `0 l5 _$ E5 C
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
' N5 a8 R' l& o: A" g" n) Hthen dilute to 1000 ml with water).2 w: f  [$ A1 D7 t: `2 r
Boil the solution for 5 min, cool it quickly to room temperature in a
* l' E( i* G/ s  b3 Vstream of running water, add 3 drops of xylenol orange TS, and mix.% y0 v8 ^( O/ F" x1 c
Using the zinc sulfate solution as titrant, titrate the solution to the first
5 [, R; s5 l/ E. U5 Zyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:4 A! [( i( _. ?" r* r
This titration should be performed quickly near the end-point by6 F6 K! Y# y* B6 j1 [
adding rapidly 0.2 ml increments of the titrant until the first colour, R( ]$ a$ q! ?6 ~
change occurs; although the colour will fade in 5-10 sec, it is the true
$ p: N% b' [' i: H7 v3 i; cend-point. Failure to observe the first colour change will result in an8 |: c& S4 S* B! W* r; m& Z- g
incorrect titration. The fading end-point does not occur at the second. A: R8 _# H+ N9 ]: c9 ?0 W& O% P
end-point.)6 j0 {, N5 S( K5 {0 Q' @: B8 j
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a  Q5 N4 g7 H) h. E; E3 ?
stream of running water. Titrate this solution, using the zinc sulfate: b( `, l" t$ i
solution as titrant, to the same fugitive yellow-brown or pink end-point
" t0 T- Y' X2 S7 ~; G8 ~as described above.8 S" }) J6 e( Z
Calculate the titre T of zinc sulfate solution by the formula:  K, @! N5 {4 h+ m% |* _. K% r2 y: q
T = 18.896 W / V% M3 i) a6 I5 P% Q% v' p& m
where
7 N- E5 o( c+ n' Q& v5 W9 aT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
& W! I# l1 Q# d" ?7 \W is the mass (g) of aluminium wire
5 v& U  G  Y* bV is the ml of the zinc sulfate solution consumed in the
3 X" I5 Z3 d" V# N1 Y8 @second titration
; D' l2 P* J5 @$ ~5 {9 @2 _18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and4 v- m: a3 s" W5 G  c
R is the ratio of the formula weight of aluminium oxide to
1 {- Z, C4 E( n0 n, _/ ~/ `$ _# l9 ~that of elemental aluminium.9 Y3 ]. `, m1 x9 c' u" ?. x. z
Sample Solution A% P" n$ Q! C7 i$ `6 B# L
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
" k2 S$ i& o/ H/ w5 A; ~glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
% N! ~7 Y8 U. ?3 b/ x* z(Note: Do not use more sodium bisulfate than specified, as an excess
: u* Y- K) b$ n/ ]3 C; oconcentration of salt will interfere with the EDTA titration later on in the
7 U8 a$ y4 g- }' F2 _procedure.) Begin heating the flask at low heat on a hot plate, and7 S$ T# Q$ m- U) ]; A3 \8 s
then gradually raise the temperature until full heat is reached.
3 G$ f2 t! Z% P8 s% c8 u9 u(Caution: perform this procedure in a well ventilated area. ) When
3 j+ H* J+ V9 _$ x; h: hspattering has stopped and light fumes of SO3 appear, heat in the full. \: F0 U' o% L: e& v- m' r
flame of a Meeker burner, with the flask tilted so that the fusion of the
# \0 k5 K* `( U! nsample and sodium bisulfate is concentrated at one end of the flask.
2 m2 r6 c& Y  @, aSwirl constantly until the melt is clear (except for silica content), but" [/ d9 F" [" E. r1 T- Q2 v
guard against prolonged heating to avoid precipitation of titanium$ I* B; ]) Y" ^  ?
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
7 L+ P: n9 l9 i+ q0 i5 bthe mass has dissolved and a clear solution results. Cool, and dilute to
0 ^* ~! e) b6 ^( v120 ml with water. Introduce a magnetic stir bar into the flask.
) {+ U+ v. [% G4 M  u9 X6 T' lSample Solution B
9 p, B+ |1 w# D5 a- D. {" C. [Prepare 200 ml of an approximately 6.25 M solution of sodium1 F1 P) X/ f* Z! q2 ^) m
hydroxide. Add 65 ml of this solution to Sample Solution A, while
% k, R* i! K% X$ G  e, @stirring with the magnetic stirrer; pour the remaining 135 ml of the7 G( L& W; X) E# [1 h8 @$ N
alkali solution into a 500-ml volumetric flask.1 n. r0 u& a( G! h7 \1 ~& k5 E
Slowly, with constant stirring, add the sample mixture to the alkali
. s& @5 q! A) E" [/ h6 i2 Ysolution in the 500-ml volumetric flask; dilute to volume with water,5 o$ ^( r+ v( \
and mix. (Note: If the procedure is delayed at this point for more than) C5 k: w+ ^7 P' \0 j& m8 m. d9 z
2 hours, store the contents of the volumetric flask in a polyethylene
& d) R' g% B8 ]! e2 Cbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
1 E  e# H- `2 _8 m% K* Zthen filter the supernatant liquid through a very fine filter paper. Label1 \/ r1 _" p& o. D, f) T
the filtrate Sample Solution B.) h* c/ ?* x3 Y  C6 t
Sample Solution C& X0 [1 a' A& D" z' b) l
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer3 V: m" ~" ]; ~! j' x8 P5 a; ~
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid: e. @0 y7 v5 r- H) s
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
9 ~1 Y/ f' z2 T' Y0 O6 ^/ ]- xM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is( G" b5 ]! p7 g' x  f
known, calculate the optimum volume of EDTA solution to be added
. n; w- Q' g* k/ [) \% s5 Hby the formula: (4 x % Al2O3) + 5.]
* v4 R, _7 A( h) m& RAdd, dropwise, ammonia solution (1 in 5) until the colour is just
% c8 N- p& N& Y6 `4 R' E& mcompletely changed from red to orange-yellow. Then add10 ml each
& `8 H5 O( i% iof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
8 E$ D5 p  B0 S+ V9 j: q" ?room temperature in a stream of running water, add 3 drops of xylenol9 @3 h( B: ~' a5 ]+ q$ _- m
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
) [2 N; E9 s: Dbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
: S$ b5 F% F$ v  lpH, a pink colour indicates that not enough of the EDTA solution has
2 h, A* e! G6 V/ K/ L) pbeen added, in which case, discard the solution and repeat this
* C( T6 N8 @) f8 X) C# |- h4 L3 Cprocedure with another 100 ml of Sample Solution B, using 50 ml,- v+ s7 n! E# w# n& C
rather than 25 ml, of 0.02 M disodium EDTA.
' Z$ v# {9 a/ q) [, `9 E! O2 _Procedure
( S: B. W2 G' dUsing the standardized zinc sulfate solution as titrant, titrate Sample
# t& V5 S$ o1 q5 m/ B) e4 ?: X3 MSolution C to the first yellow-brown or pink end-point that persists for
- L* `. M! @/ d4 G5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
: h8 U& E' H8 q3 ]4 E. K! Ytitration should require more than 8 ml of titrant, but for more accurate
: i" E2 s9 x% n4 {  wwork a titration of 10-15 ml is desirable.4 E/ \( C3 \1 b7 y6 X% V
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5" C. ?, Y; k- p" a
min, and cool in a stream of running water. Titrate this solution, using% T& ^: E3 \; K9 F
the standardized zinc sulfate solution as titrant, to the same fugitive, l" K* Y$ G# o, B1 r- J/ z# Y6 \5 P
yellow-brown or pink end-point as described above.
2 B2 C* j" a9 V" iCalculation:0 t# u+ |0 ]5 Z( n$ y) E
Calculate the percentage of aluminium oxide (Al2O3) in the sample
0 w. i% u, F& C" x" u% v2 mtaken by the formula:& D. M9 Y" q# W8 e' T6 q
% Al2O3 = 100 × (0.005VT)/S
# \. d% Z, t0 n; Kwhere
3 k3 r# ~/ S3 @2 _4 WV is the number of ml of 0.01 N zinc sulfate consumed in
  K2 r+ Q! i; C  G9 o- Pthe second titration,
( S4 {6 E% h) A3 }9 g3 Y0 NT is the titre of the zinc sulfate solution,. F. h' t7 R) p" D
S is the mass (g) of the sample taken, and: Z0 J) y5 A" X4 |/ u, f
0.005 = 500 ml / (1000mg/g × 100 ml).
( ?3 l# _" Q3 m+ @/ r; pSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
3 v: g: H! t+ V9 |4 N7 e  Oglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
7 O. `  r6 q. y! ^Heat gently over a Meeker burner, while swirling the flask, until- e* z" [7 m) ?
decomposition and fusion are complete and the melt is clear, except& z9 a  m# p0 D1 d& Z: b
for the silica content, and then cool. (Caution: Do not overheat the4 ?. c" G# z! C- d
contents of the flask at the beginning, and heat cautiously during5 d: T) K' c& p! P
fusion to avoid spattering.)+ P$ }5 k( y3 O" [' _0 [
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
3 p  `/ S% E/ l" I5 l$ pcarefully and slowly until the melt is dissolved. Cool, and carefully add
$ u! {# Y1 E" k! f7 }150 ml of water by pouring very small portions down the sides of the
$ u) I9 u+ x% ~flask, with frequent swirling to avoid over-heating and spattering. Allow& a  ~% N2 f% M4 z9 S
the contents of the flask to cool, and filter through fine ashless filter2 j7 J, C/ w) e0 I) b# G
paper, using a 60 degree gravity funnel. Rinse out all the silica from
& N! ?. R: ], I/ D- C" Nthe flask onto the filter paper with sulfuric acid solution (1 in 10).
* X, b9 E, ^& `+ }" I! ~Transfer the filter paper and its contents into a platinum crucible, dry in
1 y, A' E. |  a$ [+ f- `an oven at 1200, and heat the partly covered crucible over a Bunsen0 H2 U, p( v5 f( v
burner. To prevent flaming of the filter paper, first heat the cover from
. t' O* o6 U/ sabove, and then the crucible from below.
; C1 `/ i) V; zWhen the filter paper is consumed, transfer the crucible to a muffle/ Y3 t3 N! x( {3 M7 w
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
& P  b: j# }2 q! wweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated, }  ]5 B4 Z0 c! V, e6 }2 x
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first* R, R) A! R( ?# [/ K: `1 s
on a low-heat hot plate (to remove the HF) and then over a Bunsen" R/ a) u% j: d9 B$ L
burner (to remove the H2SO4). Take precautions to avoid spattering,
) h" ^5 V; g4 {. [5 p& kespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
1 M6 h9 H- i( k/ k6 b- k9 T" hdesiccator, and weigh again. Record the difference between the two3 A% c& i( W( z1 P5 W( p
weights as the content of SiO2 in the sample.. j, h& o" }9 x' `7 H
METHOD OF ASSAY( L! I: h  W% @7 h0 i/ ^- s
Accurately weigh about 150 mg of the sample, previously dried at 105o
& u( D9 S$ T8 o* sfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water+ D- q- t, d- y
and shake until a homogeneous, milky suspension is obtained. Add 30
  }; f/ h1 Y8 G# ], m! K2 Qml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially6 c4 h* c6 n6 I! z# u0 C$ Q
heat gently, then heat strongly until a clear solution is obtained. Cool,( g' C, T- h8 |0 Z
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric5 w9 D+ |- h& |0 x+ Z& T- \' p
acid, and stir. Add 3 g of aluminium metal, and immediately insert a1 N$ y( n; w! t$ L. {
rubber stopper fitted with a U-shaped glass tube while immersing the
/ v3 ]5 b& i6 k& }; Iother end of the U-tube into a saturated solution of sodium" N: ?$ [& l' R. o
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
/ Y' Q. t1 O4 Y+ i$ \hydrogen. Allow to stand for a few minutes after the aluminium metal
0 H) e: e. m9 v- ~7 Bhas dissolved completely to produce a transparent purple solution.
! o/ ~# _( g5 mCool to below 50o in running water, and remove the rubber stopper" f4 @. Z; q0 d. W
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate+ ]0 t$ W+ v# n5 H2 M$ U% B4 O
solution as an indicator, and immediately titrate with 0.2 N ferric- [" @$ L! Z1 x$ U5 M; z& h
ammonium sulfate until a faint brown colour that persists for 30& n- j: O! T. r7 r! e7 f# G8 ~3 ^
seconds is obtained. Perform a blank determination and make any
+ P! {( Q6 e3 F# }* A  V2 @necessary correction. Each ml of 0.2 N ferric ammonium sulfate is; C2 s, @+ w: s3 L* I* p
equivalent to 7.990 mg of TiO2.' n, d1 E0 S1 H% ?
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