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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) ; K- V8 H: E% _" ?( S: O' c
: ?+ R" e. P$ t9 M- I

' E3 B2 n% u# S% q, I5 U0 f+ CCAC关于二氧化钛(钛白粉)的使用规定2 A1 Z/ V# W& W, i; i% O3 K
GSFA Online . u9 y  u5 \  E' A
Food Additive Details
+ ?0 g& ?+ `% _/ ]  v% v( vTitanium Dioxide (171)$ F+ N" R! q4 A5 W
Number Food Category  
8 U; O3 O! h4 o  01.1.2 Dairy-based drinks, flavoured and/or fermented (e.g., chocolate milk, cocoa, eggnog, drinking yoghurt, whey-based drinks)  
* [, t# D3 ~2 y, P  01.3 Condensed milk and analogues (plain)  / a. T& T9 d6 [! Y, z
  01.4.3 Clotted cream (plain)  5 p# e4 A: R; o5 M( W
  01.4.4 Cream analogues  
$ L& d  x  W5 W. d  01.5 Milk powder and cream powder and powder analogues (plain)  
# ?7 b  c. W. g2 p2 c9 [1 T+ i$ d  01.6 Cheese and analogues  
, i. ?$ r7 X# @; X) {$ m5 N  01.7 Dairy-based desserts (e.g., pudding, fruit or flavoured yoghurt)  
+ s' S* z% O* ]( V  01.8 Whey and whey products, excluding whey cheeses  
4 I5 I' t# G5 C; w4 U) n  02.2.1.2 Margarine and similar products   $ C0 X0 V0 x2 A( Z7 O, v
  02.2.1.3 Blends of butter and margarine  - r. T1 N2 s5 h6 H. x5 l. c
  02.2.2 Emulsions containing less than 80% fat   
" Q" x& U& ]* P& y. Q; ?' F0 Q3 b  02.3 Fat emulsions maily of type oil-in-water, including mixed and/or flavoured products based on fat emulsions   
1 D  n6 F' {% L; V* w2 p3 t6 o  02.4 Fat-based desserts excluding dairy-based dessert products of food category 01.7  ! b0 C) D" m( c; L
  03.0 Edible ices, including sherbet and sorbet  : ~2 l; k) u7 k1 m
  04.1.2 Processed fruit  
% L0 A7 Z/ S) `1 J- \  04.2.2.2 Dried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweeds, and nuts and seeds  
! [5 e% V/ }# u; h9 J' U- C  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  $ n3 {. ]9 N8 w. ~6 I/ u
  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  
8 x9 \. P$ P- e7 D; m* x3 x$ 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)  
3 P' p7 h/ `0 Y, d4 d0 P  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/ }! W- `, o. |- {3 ~  04.2.2.8 Cooked or fried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  
. r: k# q" L% D. B$ ~  05.0 Confectionery  9 O/ u* ]7 P# v% F4 N+ _; C
  06.3 Breakfast cereals, including rolled oats  
, i9 ^4 H) g7 H) S. D  06.4.3 Pre-cooked pastas and noodles and like products  
/ T* G# G$ ?3 N& }  06.5 Cereal and starch based desserts (e.g., rice pudding, tapioca pudding)  & f& \; W8 N7 U3 p. [7 ?8 _+ d
  06.6 Batters (e.g., for breading or batters for fish or poultry)  $ |" V7 A6 F1 h3 h1 a5 {+ V
  06.7 Pre-cooked or processed rice products, including rice cakes (Oriental type only)  
: O: l# [9 M4 Y1 U* ]" D  06.8 Soybean products (excluding soybean products of food category 12.9 and fermented soybean products of food category 12.10)  4 S) {7 A4 n7 c/ R: |6 _+ Z1 @1 O
  07.0 Bakery wares  
, y4 {; P) }2 H% w3 k  08.2 Processed meat, poultry, and game products in whole pieces or cuts  6 {, v9 j+ Z+ B5 {
  08.3 Processed comminuted meat, poultry, and game products  ; i' c' N- x+ t6 @/ ?
  08.4 Edible casings (e.g., sausage casings)  & O1 a" ]" w6 P( @1 d
  09.3 Semi-preserved fish and fish products, including mollusks, crustaceans, and echinoderms  . F9 m4 O" S& J/ y! u0 u8 `
  09.4 Fully preserved, including canned or fermented fish and fish products, including mollusks, crustaceans, and echinoderms  
4 u( }$ h5 s6 f& n: A7 ^  10.2.3 Dried and/or heat coagulated egg products  / j9 o% f2 d( A5 l, r, ?( c" m
  10.3 Preserved eggs, including alkaline, salted, and canned eggs  
% l1 J1 C" ]  @" z; d% l5 n, i  10.4 Egg-based desserts (e.g., custard)    E% l1 @3 N, s
  11.6 Table-top sweeteners, including those containing high-intensity sweeteners  
+ O8 D% H0 G7 B4 ^2 Z$ J  12.2.2 Seasonings and condiments  
+ b( ]6 d1 e( p; E  12.3 Vinegars  
" R5 C- `/ n8 B( }, ^  12.4 Mustards  
& Q$ D& L' {, I7 G: |+ B  12.5 Soups and broths  
2 ?( m2 g5 n2 p2 Z. z# x; K  12.6 Sauces and like products  
% q5 z/ `) t2 a9 D3 Z  Y, |4 l  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  
8 n* E/ a% ]0 U! f& x. j5 h  12.8 Yeast and like products  
: e% T/ c0 V1 J( S6 }* w  12.9 Protein products  
3 p, a2 w0 Q& u' g' C9 e; y  12.10 Fermented soybean products  - P' T" r5 d! j1 e2 L% i9 u; `2 p
  13.3 Dietetic foods intended for special medical purposes (excluding products of food category 13.1)  ' X6 w# b0 O; q4 H9 k( U& @( K
  13.4 Dietetic formulae for slimming purposes and weight reduction  
2 C! w& ^# ?5 h" F8 e& w! y* z  13.5 Dietetic foods (e.g., supplementary foods for dietary use) excluding products of food categories 13.1 - 13.4 and 13.6  2 l8 [3 h. C% m7 \/ s( a+ _5 K# r
  13.6 Food supplements  8 Q$ l  p+ p& @+ a0 O
  14.1.1.2 Table waters and soda waters  
% F) [+ k. [5 }* W3 |  14.1.4 Water-based flavoured drinks, including "sport," "energy," or "electrolyte" drinks and particulated drinks  # i: R+ b8 }" @) E) A
  14.2.1 Beer and malt beverages  
4 e1 G4 A% Z. T+ p4 s& N  14.2.2 Cider and perry  
1 a9 H, d' v1 G' {  14.2.4 Wines (other than grape)  , I. a/ i' r9 ^  [* L1 x# [
  14.2.5 Mead  ( j3 |0 x" b7 t' o7 Z4 C
  14.2.6 Distilled spirituous beverages containing more than 15% alcohol  ! ]+ C* O$ i( w# p6 `8 P$ m
  14.2.7 Aromatized alcoholic beverages (e.g., beer, wine and spirituous cooler-type beverages, low alcoholic refreshers)  % y* d0 M6 N7 G8 _& h, Y
  15.0 Ready-to-eat savouries  1 Z9 E3 V, Y( [
  16.0 Composite foods - foods that could not be placed in categories 01 – 15
/ U6 Z, H' N) t- ^2 ^8 X$ A% u: R9 P& M/ A! _& v0 h. r; t' L

. Y) }0 Q: R6 J部分译文:
8 `5 W& N' c4 G$ o0 N/ {4 D( Q. V' g6 |/ R3 }, U
食品添加剂通用规则9 I( w6 S& Y- i4 w  G, l
食品添加剂, X0 v# G3 j5 e9 |6 y+ s2 Q& ]
                    二氧化钛(171)& v7 W; N( z* C; q' e/ d/ E
食品类别:" g8 s6 ^; c& e, g4 l
06.3 早餐谷类,包括燕麦片
2 t( q7 a2 n* s) [06.4.3面条及类似产品
$ x, t( z! H: F% z06.5 谷类,淀粉甜点(包括:米粉布丁,木薯布丁)  D( D, q; o& h& h/ T
06.6 面团3 k. g% `8 {6 s9 i4 N  I; e0 N4 _
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
! W- H2 ^/ k  i. X07.0 烘焙类
+ |- V" ?3 d% F8 m8 ^  I9 b07.1 面包,普通烘焙类,以及其混合物
  X4 d& L3 x" ]5 Q, m4 Q- I$ e07.1.1 面包,面包卷
- c1 q$ S8 q6 d2 u07.1.1.1 酵母发酵面包及特殊面包1 I/ Z" {2 n2 I6 _
07.1.1.2 苏打面包
. {. Z6 k6 `6 _! Z* h' r( ~! M/ Z) w
; a& |) G0 T! k  N$ r! j
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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)+ X2 S/ ^, A- n! ?/ P; E6 o* y3 `
, ?. P3 w1 B/ H  t5 l
JECFA关于二氧化钛(钛白粉)的结论
0 |% m9 e  b" J% {" y- u0 Y( \1 M, F- `8 k' d9 B5 C
摘要: 2006年JECFA关于二氧化钛的结论5 b2 e) p' a9 I) o3 J( d
ADI值:不作限制。
( C. h! ~1 Z) ~7 A3 d. W! J/ w功能:着色剂- p+ }9 z' x  L( H$ `. v

: [* {/ Y- H4 A5 f7 y7 ~5 [TITANIUM DIOXIDE0 I9 ]2 f6 ]& V5 e" V4 r5 E) S
Prepared at the 67th JECFA (2006) and published in FAO JECFA9 P) ~5 {4 k& d
Monographs 3 (2006), superseding specifications prepared at the 63rd
9 Y$ ~" n4 h2 z* IJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
( b6 k5 U8 t5 g1 `Combined Compendium of Food Additive Specifications, FAO JECFA# W- A  s- _+ ]" m" u# J) G2 l
Monographs 1 (2005). An ADI “not limited” was established at the 13th7 o* |! V# u, ~8 d* C$ t* T
JECFA (1969).; r: b6 R, G8 M2 I- I& R+ N
SYNONYMS" }' x4 O3 X+ @( Y7 Y1 Q
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
( b* h8 V, k# \  [4 EDEFINITION& t% N) H) p% c5 L- O
Titanium dioxide is produced by either the sulfate or the chloride7 K  G' Y1 ~% y- l) i1 N
process. Processing conditions determine the form (anatase or rutile
0 ]+ j9 F& z* p8 ^" pstructure) of the final product.
' T/ r* D+ L# hIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)4 p# Q9 T4 r/ i9 F
or ilmenite and titanium slag. After a series of purification steps, the7 w% _& o$ @1 d$ ?
isolated titanium dioxide is finally washed with water, calcined, and
. k, F0 u: a5 ?micronized.
6 _8 n  U: \$ X) m, N- h9 f' sIn the chloride process, chlorine gas is reacted with a titaniumcontaining
) v6 E( A! I! c. V& p1 g/ `. Imineral under reducing conditions to form anhydrous1 F1 t  F: {' d* Q1 W) k
titanium tetrachloride, which is subsequently purified and converted to
8 Z) u' ]: U8 c: C4 Ftitanium dioxide either by direct thermal oxidation or by reaction with
. D. d& H3 E* N1 H5 Lsteam in the vapour phase. Alternatively, concentrated hydrochloric
- |: N( B) ]  n* o/ I0 J, Vacid can be reacted with the titanium-containing mineral to form a
5 G5 Y* v+ R2 b8 I: vsolution of titanium tetrachloride, which is then further purified and0 }/ h7 J: F+ n( s" k1 S
converted to titanium dioxide by hydrolysis. The titanium dioxide is
* I& T5 w6 n: V/ b7 kfiltered, washed, and calcined.
& l# H- R3 r2 O4 j" BCommercial titanium dioxide may be coated with small amounts of1 T) W  }* M4 Y  Z, l
alumina and/or silica to improve the technological properties of the, W0 l. M0 H/ i; _7 z/ ^* v$ \0 q
product.- k2 R" y% t( I; J, {0 O. C
C.A.S. number 13463-67-7
7 b' b# ^# Z' W5 M9 F! GChemical formula TiO20 {) ]0 f% |9 a% k6 F
Formula weight
9 a3 f- N, t, l1 o8 H) b* U9 b79.88
- \, Z: O5 C* C# g$ B( h' F$ ZAssay& v/ D3 t7 ?3 l( l& [
Not less than 99.0% on the dried basis (on an aluminium oxide and3 O2 l: m2 u  _, u2 K, J" K) Q
silicon dioxide-free basis)
/ |" ]9 z  u$ f8 E: }4 P9 SDESCRIPTION
8 p: Z& {+ F/ H7 E! S, l1 QWhite to slightly coloured powder
) M$ w2 F8 t) C* j. ZFUNCTIONAL USES
* Q/ F# B1 Z" ~6 DColour: I. K6 S4 Q3 v! N/ P
CHARACTERISTICS
4 U1 }" Z) t1 e) j" F9 r# v) WIDENTIFICATION' g( t+ T' b. [8 F" F7 B# z2 W
Solubility (Vol. 4)
/ z, f/ {6 q2 W- `& K0 _( F0 FInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
3 F' ?( ~: ?% [( o; h) T8 {solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
8 c% _+ S0 F6 N: f3 u0 ysulfuric acid.% J/ z6 O+ i# Z: _* J
Colour reaction. X1 d0 d) e/ k3 H0 h
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
" ~# A4 L: o5 D8 p3 p; x( Z! asulfuric acid appear, then cool. Cautiously dilute to about 100 ml with6 W5 n& _" d  G2 ^9 c
water and filter. To 5 ml of this clear filtrate, add a few drops of
. Q5 G& E6 o6 g% Z" e& thydrogen peroxide; an orange-red colour appears immediately.  `- S6 b. `. y0 C2 U
PURITY& g( W5 s) d8 E% z: ^$ a+ Y! Q
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
/ n% Q* U! e0 t) n0 hLoss on ignition (Vol. 4)" H$ m  Y# r% z& b6 d
Not more than 1.0% (800o) on the dried basis
1 |. h* ~/ F' C' z* r5 TAluminium oxide and/or4 H* E. ~$ d  f3 z+ H- @
silicon dioxide
; Y3 V8 o0 {2 B' n* ^Not more than 2%, either singly or combined) j) g- n) n6 O3 S2 W
See descriptions under TESTS
  ?/ O  V, F' ^1 `0 r! Z0 N$ yAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing: D+ F5 H8 r7 j# u
alumina or silica.7 E+ O- c' b, ?4 |1 o/ B- x
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
: b+ z' d9 g7 n4 [) Bplace on a steam bath for 30 min with occasional stirring. Filter7 _6 F' i( X7 ^
through a Gooch crucible fitted with a glass fibre filter paper. Wash1 d5 A0 ^; N6 N$ f* V
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
: I- }4 i) G- ccombined filtrate and washings to dryness, and ignite at a dull red
+ @9 N0 W& s" Z  S) |heat to constant weight.
$ d( u; t: m/ b6 r. ZWater-soluble matter- _8 K; ]% e% t3 U; h
(Vol. 4)
3 ]. ^  U* ~+ Q2 |6 JNot more than 0.5%
9 Q, {# q+ i* c! E* F8 pProceed as directed under acid-soluble substances (above), using
( T& c) X. n) I! s2 d9 bwater in place of 0.5 N hydrochloric acid.
; ]4 X+ C" o1 `: Z( QImpurities soluble in 0.5 N$ l2 U( {( M. v9 P) d. k+ Q
hydrochloric acid$ p* ?; N+ L- d& h
Antimony Not more than 2 mg/kg( }4 p; B7 c( `! p2 N: v
See description under TESTS. l; t6 D4 r6 y& e4 I; u) v1 k& y, K% v
Arsenic Not more than 1 mg/kg; Z2 v' z3 f4 W! d5 h
See description under TESTS' P+ Z7 b) Y4 O3 G6 j, W
Cadmium Not more than 1 mg/kg; b4 i4 W0 I. u  N# p" ^! |, n
See description under TESTS' b# {0 X( g; {& R2 ]2 C( {: g
Lead! R- ?$ ]/ ~: ~$ U8 s/ J4 Q9 U, K
Not more than 10 mg/kg  ?. _- H1 k* q
See description under TESTS
3 c) V4 P0 X' v" R5 t1 `# ^Mercury (Vol. 4) Not more than 1 mg/kg8 o8 U6 U% ?7 Q8 X0 z9 c% {2 ^
Determine using the cold vapour atomic absorption technique. Select a
0 Z0 t" f+ h) u( a' asample size appropriate to the specified level
; B& F2 L+ C0 T0 p: i! ?; yTESTS
% k& M$ n6 K6 r* ^% ?# J7 RPURITY TESTS
" E: C) S7 l4 N0 AImpurities soluble in 0.5 N, m- x) L9 w4 s- L% J2 I* _
hydrochloric acid2 M5 m! C" O. e# ?4 ]! B
Antimony, arsenic,
+ s( J6 ~3 s" V7 B) g+ P4 rcadmium and lead/ |2 C9 O2 }, I4 |5 f4 v. M5 R/ {
(Vol.4)- n2 v9 Q, v: r" A0 g# C
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
# a" ?0 N* I% c7 p" z% O1 _5 _hydrochloric acid, cover with a watch glass, and heat to boiling on a
; P9 c6 V- ^# x! s4 d( f! E# _hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml! S% t+ m% J0 G# j. O' G9 f* J9 A
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved7 _+ o  I/ h3 q3 I* r: s
material settles. Decant the supernatant extract through a Whatman
- k3 g) e2 l" T+ R- I. {) N7 a6 UNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml4 F' R$ y6 d( l& h. U  l
volumetric flask and retaining as much as possible of the undissolved
% f  c, o- `8 }) zmaterial in the centrifuge bottle. Add 10 ml of hot water to the original- ?7 O6 l4 q0 S% O$ r: R3 R
beaker, washing off the watch glass with the water, and pour the
9 o5 u; A2 c* \$ I- econtents into the centrifuge bottle. Form a slurry, using a glass stirring4 J- `' ]8 c: m1 R' [) z7 E
rod, and centrifuge. Decant through the same filter paper, and collect
4 g( V% O. _: R  [the washings in the volumetric flask containing the initial extract.. E2 y/ l$ g- @6 C. e
Repeat the entire washing process two more times. Finally, wash the6 ]. I9 h% S; B0 V  l, X3 g
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask- @1 h: h% p1 q" f
to room temperature, dilute to volume with water, and mix.7 d( G% b& E2 h0 W" ^
Determine antimony, cadmium, and lead using an AAS/ICP-AES; @& j, }: Z' u& r# y
technique appropriate to the specified level. Determine arsenic using the$ X" i9 n& `8 R; q2 [
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
& ?& l) r, U8 F2 mMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than/ v) N1 a! y# x- |$ e0 L
1 g. The selection of sample size and method of sample preparation
0 ~) ]% O* V+ f; u  {may be based on the principles of the methods described in Volume 4.
% U5 ]$ b4 i) a; Y$ r0 nAluminium oxide Reagents and sample solutions# w# |9 N5 k' G; h) Y
0.01 N Zinc Sulfate
% s. _& n! A2 g. L" O: i, F( p$ QDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
) q/ l8 b9 ]9 d2 e7 ]; A! _2 Gmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
5 W- t  `4 t8 R8 Wof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
6 p+ `0 G- C1 @3 Lconcentrated hydrochloric acid, heating gently to effect solution, then. {% V' h# J. p: l" V
transfer the solution into a 1000-ml volumetric flask, dilute to volume3 _' x1 r" F6 e+ h0 `9 G. I6 {) G
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
! Q$ I. O9 t1 {- r; n& h) M3 ]3 Fml Erlenmeyer flask containing 90 ml of water and 3 ml of
; \- J' P! V2 ?concentrated hydrochloric acid, add 1 drop of methyl orange TS and
! q9 c( K5 T$ C/ y25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
+ y5 j: u5 W; S& tdropwise, ammonia solution (1 in 5) until the colour is just completely
: k$ n* ?4 R5 S$ \0 ^4 S0 Schanged from red to orange-yellow. Then, add:
. W4 h" H/ O6 c8 q) X; ~1 O(a): 10 ml of ammonium acetate buffer solution (77 g of
$ Q& r% V8 }5 L5 f; X4 y- Cammonium acetate plus 10 ml of glacial acetic acid, dilute to
4 m1 ]* f5 i. v1000 ml with water) and
& L0 L4 o5 @$ m9 V0 [/ O0 `  E(b): 10 ml of diammonium hydrogen phosphate solution (150 g
: f8 _% d  V! G& c4 uof diammonium hydrogen phosphate in 700 ml of water,
8 t* H. x4 N& q8 x7 Y# z( y, m/ Badjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
/ ^1 j, Z+ N+ ~: C7 Rthen dilute to 1000 ml with water).
5 u6 @7 G* h2 o/ x/ W8 k  CBoil the solution for 5 min, cool it quickly to room temperature in a" ~5 [/ |( F; o. K0 {
stream of running water, add 3 drops of xylenol orange TS, and mix.
1 J- P+ I5 M0 G) I. d- M3 VUsing the zinc sulfate solution as titrant, titrate the solution to the first
! C; U" ^: Y4 ~# |0 b$ {yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
! r; k3 \$ E+ F% `This titration should be performed quickly near the end-point by
' E+ w: K' p1 Uadding rapidly 0.2 ml increments of the titrant until the first colour
5 [! M! V+ o9 l  ]& M4 P3 [change occurs; although the colour will fade in 5-10 sec, it is the true
% a; E! C. ]7 ^6 I2 F! M4 g) Send-point. Failure to observe the first colour change will result in an
0 \2 E1 ^* Z! ^  ~6 X; ]incorrect titration. The fading end-point does not occur at the second7 _, X/ U, U1 p3 L. H
end-point.)
, I+ P( |) m3 L+ {' v$ A9 `- Z' OAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a. }1 g2 H( G, W
stream of running water. Titrate this solution, using the zinc sulfate
5 V# {& |1 p$ X4 z+ Y3 u! {0 osolution as titrant, to the same fugitive yellow-brown or pink end-point
+ M# }; l5 f; Y; s5 Mas described above.! x# ~2 U) B7 b. X: a; `) V0 H
Calculate the titre T of zinc sulfate solution by the formula:/ `" X4 W( Y( @0 ~; t
T = 18.896 W / V" ~1 V& [! f# l, J
where9 w8 Y5 L/ I! z8 C
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution) n' Q& T- k/ s( X2 Q) i/ P
W is the mass (g) of aluminium wire- N% O( X, x+ s4 Y$ s
V is the ml of the zinc sulfate solution consumed in the
; e- ~4 s. r- N& x6 E1 L  |0 i& esecond titration. u6 \. A4 u2 b: f! I0 W
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and8 h$ a& c) O5 n+ F8 X
R is the ratio of the formula weight of aluminium oxide to+ @& @( h3 B/ Z6 i
that of elemental aluminium.. k$ j; L2 Y" {  M" H3 |% N: q
Sample Solution A" h: I& m* g8 S5 N- C7 V; e5 Z
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
$ W3 R5 l* h* Y0 [* G4 C* `) fglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
7 o# ?) \+ _# K0 n(Note: Do not use more sodium bisulfate than specified, as an excess
  E5 d1 o! p; r- sconcentration of salt will interfere with the EDTA titration later on in the
8 i* h% F3 Q) p$ Hprocedure.) Begin heating the flask at low heat on a hot plate, and/ C1 l+ v: m$ H3 ?; u
then gradually raise the temperature until full heat is reached.$ j3 }) x8 u3 A+ i) C6 C
(Caution: perform this procedure in a well ventilated area. ) When
9 D9 {; J' p0 z3 r2 Z; l' ispattering has stopped and light fumes of SO3 appear, heat in the full
; D" u6 W+ w$ V7 q" J* Sflame of a Meeker burner, with the flask tilted so that the fusion of the
6 T- W# }: ^' isample and sodium bisulfate is concentrated at one end of the flask.
' E5 `$ \0 F. W3 y' ^5 X, oSwirl constantly until the melt is clear (except for silica content), but1 v( W$ W& f- _
guard against prolonged heating to avoid precipitation of titanium4 ?9 @$ U/ e0 |3 M' Y7 f+ q
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until/ T- t0 w; J- R. t) y9 ?0 j
the mass has dissolved and a clear solution results. Cool, and dilute to
# y) M8 R0 _7 O# R+ m" N5 p- r  u120 ml with water. Introduce a magnetic stir bar into the flask.
$ y  [; c: l8 `0 e6 ~! xSample Solution B# _* K  x$ }- u7 D& X' E- o
Prepare 200 ml of an approximately 6.25 M solution of sodium
# V& Z' C  V3 D. |% [; q' P9 I. ahydroxide. Add 65 ml of this solution to Sample Solution A, while
1 a0 S$ s& W( M0 I6 T: v/ @6 y1 ?stirring with the magnetic stirrer; pour the remaining 135 ml of the1 O: d0 z3 j5 D! R& |
alkali solution into a 500-ml volumetric flask./ g* f( X2 \, b7 @
Slowly, with constant stirring, add the sample mixture to the alkali
, G+ n3 m# M6 h6 K0 X" Osolution in the 500-ml volumetric flask; dilute to volume with water,
- j  D& s( f% M( rand mix. (Note: If the procedure is delayed at this point for more than  N% f' I6 n6 \/ B, ~  A' p
2 hours, store the contents of the volumetric flask in a polyethylene
  Q/ J; ~2 |- d, gbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),  u# j$ ^# G; E2 `" r
then filter the supernatant liquid through a very fine filter paper. Label. [1 D' C) w" Q- D) S9 R  T
the filtrate Sample Solution B.- ~* S$ T# r; w1 `
Sample Solution C- M* y* s% `. V2 ?
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
" T1 K: W1 X) ^$ C: G  U- P) vflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
; x7 y* K3 Q' j5 Z  Jsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
' ^" u( y7 o/ [, p/ a% `( gM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
/ E7 q1 f' H) j) aknown, calculate the optimum volume of EDTA solution to be added
7 `8 Y4 z7 J$ d5 d: }) k: S4 d# qby the formula: (4 x % Al2O3) + 5.]) |6 p2 [7 D7 r4 }" e! U& {, ]
Add, dropwise, ammonia solution (1 in 5) until the colour is just
' i# j1 o8 D/ D; Y" |completely changed from red to orange-yellow. Then add10 ml each
1 c' x7 D( m+ ?6 _of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to% n: T  l/ Z1 T: Z" w
room temperature in a stream of running water, add 3 drops of xylenol
, E0 [0 J% {6 n2 h" {orange TS, and mix. If the solution is purple, yellow-brown, or pink,) w; d  o$ ?! U$ p  x' p* K
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired+ P; R& P* L  r+ v: g5 f& ~, u
pH, a pink colour indicates that not enough of the EDTA solution has
- w# G7 C: R+ zbeen added, in which case, discard the solution and repeat this7 U  ?; G/ \3 B0 ~
procedure with another 100 ml of Sample Solution B, using 50 ml,
; r0 }% b( C$ T' Trather than 25 ml, of 0.02 M disodium EDTA.
" r, t* r) _  |+ I2 j' }' j0 _Procedure
) `2 e2 C( t: S9 u/ t3 V  x* mUsing the standardized zinc sulfate solution as titrant, titrate Sample/ W. ]+ S1 @' j  j( a
Solution C to the first yellow-brown or pink end-point that persists for
9 @4 ?7 p; t7 @7 p4 c5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
' S2 {  v' ?: rtitration should require more than 8 ml of titrant, but for more accurate
% m8 Y0 D9 ^# R) ^. z5 Y) Pwork a titration of 10-15 ml is desirable.! o! m" t6 A9 m6 T. [6 m
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
) }$ c3 Y9 ~3 `6 w3 b( Omin, and cool in a stream of running water. Titrate this solution, using5 a; U' p; x6 l5 W1 t3 t. G5 j
the standardized zinc sulfate solution as titrant, to the same fugitive& L  ~9 L9 z5 e
yellow-brown or pink end-point as described above.# ]1 C: H; _4 {# N
Calculation:$ a8 M) f/ |; B7 h9 ^' m7 `6 U
Calculate the percentage of aluminium oxide (Al2O3) in the sample- X: @8 {3 X( ]
taken by the formula:
+ j5 I: f- m* J. ]- M% Al2O3 = 100 × (0.005VT)/S
7 h4 _+ \  ?% J: a, l8 gwhere8 x- O& t. C& A3 P" c
V is the number of ml of 0.01 N zinc sulfate consumed in
$ _1 |- D: [, P& V  Ethe second titration,
4 H' h" b" {9 V5 ~9 r, Z4 eT is the titre of the zinc sulfate solution,
$ ?, S- }+ w8 L% dS is the mass (g) of the sample taken, and
  h( h  T6 T+ I5 K* X9 w0.005 = 500 ml / (1000mg/g × 100 ml).3 w, d$ G- Z& G/ R4 F
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica: [$ ]% }2 e& Z; x# D7 R
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).; Z8 {' l- q% _8 x
Heat gently over a Meeker burner, while swirling the flask, until5 [1 o+ ]6 p4 Y4 G
decomposition and fusion are complete and the melt is clear, except* w1 f3 k+ b( x# H' @& T
for the silica content, and then cool. (Caution: Do not overheat the
6 q" F  b0 S1 H- K# |( R8 ^contents of the flask at the beginning, and heat cautiously during4 I3 a1 Q# g( s5 g' c6 _, M' j3 m+ a
fusion to avoid spattering.)
( E# _  S; {5 e" F0 `To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
4 n1 }: e: ?! d, Xcarefully and slowly until the melt is dissolved. Cool, and carefully add# M1 e- R! t& y+ x) w% d  W
150 ml of water by pouring very small portions down the sides of the5 O2 X( l* T$ U8 o9 r
flask, with frequent swirling to avoid over-heating and spattering. Allow
" d5 B* ]: w1 u. X3 |- G! Xthe contents of the flask to cool, and filter through fine ashless filter
" F9 M2 @' ]4 Y/ [/ epaper, using a 60 degree gravity funnel. Rinse out all the silica from, A, T# M  y; }+ C
the flask onto the filter paper with sulfuric acid solution (1 in 10).
' k4 N5 _- M0 O; e* I6 I( nTransfer the filter paper and its contents into a platinum crucible, dry in
# T0 g/ Z  S2 [  E- Yan oven at 1200, and heat the partly covered crucible over a Bunsen. [9 L9 X$ E: [, \/ ^% S0 n
burner. To prevent flaming of the filter paper, first heat the cover from2 K9 ^- q, Y' o0 b& K
above, and then the crucible from below., q& y1 z! [( _( [- J
When the filter paper is consumed, transfer the crucible to a muffle
% O) G2 ]# j, F! \+ yfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
- B& O: B+ `4 O3 O% S2 A+ fweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated  \# {  y, ?4 H3 R0 H6 j) G7 H6 ]
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first; B: v5 _: m8 ~1 O1 a
on a low-heat hot plate (to remove the HF) and then over a Bunsen6 g0 u# ~* C: S/ D7 z; |3 V
burner (to remove the H2SO4). Take precautions to avoid spattering,! l7 q: C! M- e8 g: n
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a+ V% p$ |5 a, M7 U0 \9 {% Y& @/ O
desiccator, and weigh again. Record the difference between the two
: ]2 Z( q4 R( x' `$ [) l8 \: Tweights as the content of SiO2 in the sample.0 j, {2 d; b& p6 d5 \7 E' v
METHOD OF ASSAY( w2 A: |7 U; E3 d5 {! O$ `
Accurately weigh about 150 mg of the sample, previously dried at 105o1 ]: s9 F! ~! Z  d
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
, t5 H/ X+ u3 y9 I5 h" `and shake until a homogeneous, milky suspension is obtained. Add 30
! S9 `: W: n! `4 [/ Nml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially  @8 D; W( ^3 M2 W8 d
heat gently, then heat strongly until a clear solution is obtained. Cool,# V2 H% ~( Z6 W% C
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric6 O$ q3 ~6 _+ w4 g
acid, and stir. Add 3 g of aluminium metal, and immediately insert a3 z' K1 t+ T! |' B/ U" A3 v- P9 |
rubber stopper fitted with a U-shaped glass tube while immersing the! ]0 r$ O4 e( S3 ?
other end of the U-tube into a saturated solution of sodium/ v/ e9 b. X, U
bicarbonate contained in a 500-ml wide-mouth bottle, and generate9 T4 o5 C! P4 t
hydrogen. Allow to stand for a few minutes after the aluminium metal# ?: x& Y8 S! `- k% Z0 U
has dissolved completely to produce a transparent purple solution.( G/ M  d) O! ~& G& J
Cool to below 50o in running water, and remove the rubber stopper4 ~% e/ O% p' @5 J# Q# N. d
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
" S$ \; e& f  Y/ Z% S8 esolution as an indicator, and immediately titrate with 0.2 N ferric0 p: z# W* V) Y
ammonium sulfate until a faint brown colour that persists for 30
  @- t: ?/ Q* u/ }1 t% B8 ~3 Nseconds is obtained. Perform a blank determination and make any1 \* R* \1 B: I! |" ~3 o" b
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
2 K  U  Q- l/ Z" B( }- [) iequivalent to 7.990 mg of TiO2.( F: f/ I1 v5 ^7 J- d) r) @
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