2 S n 2 + C r % 1[4] % [5] % 100ms [ 6 ] 1 0 µ A 10-8 mol 100% 3 T i +

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1 10 - ph - Szebelledy Somogy[1] DL5x DL7x A. De Agostini Q - DL38 DL39 m[g ] M Q - m = z F - ph M [g/mol] F C/mol z Seven 1917 Grower[2] [ 3 ]

2 2 S n 2 + C r % 1[4] % [5] % 100ms [ 6 ] 1 0 µ A 10-8 mol 100% 3 T i +

3 Pt/NaBr As(III) U(IV) NH 3 SO 2 H 2 S Fe(II) Pt/KI H 2 S SO 2 As(III) Sb(III) Pt/NaCl As(III) Fe(II) (IV) Pt/Ce 2 (SO 4 ) 3 U(IV) Fe(II) Ti(III) I - (III) Pt/MnSO 4 Fe(II) H 2 O 2 Sb(III) (II) Pt/AgNO 3 Ce(III) V(IV) H 2 C 2 O 4 (II) Pt/Fe 2 (SO 4 ) 3 Mn(III) Cr(VI) V(V) Ce(IV) U(VI) Mo(VI) (III) Pt/TiCl 4 Fe(III) V(V, VI) U(VI) Re(VIII) Ru(IV) Mo(VI) (II) Au/SnBr 4 (NaBr) I 2 Br 2 Pt(IV) Se(IV) (I) Pt/Cu(II)(HCl) Fe(III) Ir(IV) Au(III) Cr(IV) IO 3 (V) (IV) Pt/UO 2 SO 4 Cr(VI) Fe(III) % (II) Hg/CrCl 3 (CaCl 2 ) O 2 Cu(II) (I) Ag/HClO 4 S 2- (I) Hg/NaClO 4 EDTA Hg/HgNH 3 EDTA 2- Pt/Ag(CN) Ni(II) Au(II, I) Ag(I) Pt(-)/Na 2 SO 4 CO 2 Pt(+)/Na 2 SO 4 CO 3 NH D L [4] [7] D L 3 9 ROH + SO 2 + RN (RNH)SO 3 R 2RN + (RNH)SO 3 R + I 2 + H 2 O (RNH)SO 4 R + 2(RNH)I

4 [1] L. S ze be l le d y an d Z. 5 0 Somogyi, Z. anal. Chem., 112, 313, 323, 332, 385, 391, 395, 400 (1938) DL39 [2] G. G. Grower, Am. Soc. Testing Materials, Proc., II, 17, (1917) [3] James J. Lingane, Electroanalytical Chemistry, Sec ond Edition, Interscience Publishers (1958) [mg/100g] [4] A. J. Bard, L. R. Faulkner, Electrochemical Methods, Second Edition, Wiley (2001) [5] Paul Delahay, New Instrum e n t a l M e t h o d s i n DL32 DL39 E l e c t r o c h e m i s t r y, Interscience Publishers (1954), p.304 G L P [6] E. Eisner et.al., Analytica Chimica Acta 359 (1998), DL32 DL39 -[7] E. Scholz, Karl Fischer Titration, Springer-Verlag Berlin (1984) p p m 5 % DL DL32 DL39 DL32 DL

5 DL5x DL7x P. Gilmer - DL5x DL7x 0 H 1 0 Sample 3 0 H 2 R Stir Titra- tion Calculation DL7x 1 [ H 2 ] DL5x DL7x 5... n 20 H1...H20 Sample [ H 1 ] 2 [H1=H1+1] 3 [H2=R1] [H1] [ H 1 ] 2 T i t l e Sample C a l c u l a t i o n 1 [R2] [H1]

6 6 Title Method ID Title... Acid number Date/time Reb :48 pm 1. Auxiliary value ID test... Counter set to zero Formula... H1=0 Sample Number samples Titration stand... ST20 1 Entry type... Fixed volume U Volume [ml] ID1... AN01 Molar mass M Equivalent number z... 1 Temperature sensor... Manual 2. Auxiliary value ID test... Counter plus one Formula... H1=H1+1 Stir Speed(%) Time(s) Titration Titrant... 1/2 H2SO4 Concentration[mol/L] Sensor... DG111-SC Unit of meas... As installed Titration mode... EP Titrant addition... Dynamic de(set)[mv] dv(min)[ml] dv(max)[ml] de(mv) dt(s) t(min)(s) t(max)(s) Delay (s)... 0 End point mode... EPA Potential[mV,pH...] Tendency... Negative Maxmium volume[ml] Calculation Result name... Acid number Formula... R=VEQ*10 Constant... Result unit... g/l Decimal places Auxiliary value ID test... Save result Formula... H2=R1 Condition... Yes Condition... H1=1 4. Calculation Result name... Average Formula... R2=(R1+H2)/2 Constant... Result unit... g/l Decimal places... 3 Condition... Yes Condition... H1=2 5. Auxiliary value ID test... Counter set to zero Formula... H1=0 Condition... Yes Condition... H1=2 Statistics Ri(i=index)... R1 Standard deviation s... Yes Rel.standard deviation srel. Yes Record Output unit... printer + computer All results... Yes

7 4 [ H 1 ] [H1} DL5x DL7x 0 - Rondo Sample Statistics SU24 7

8 DL38 DL39 A S T M - - DL3 8 DL3 9 DL39 - DL38 - DL3 8 DL3 9 DL39 D L 3 8 DL38 DL39 x RSD 1.0g mgbr/100g 1.91% SH/T0630 DL39 0.5g mgbr/100g 1.62% SH/T0630 DL39 10uL 3.32 gbr/100g 2.01% SH/T0630 DL39 5uL 9.29 gbr/100g 1.34% SH/T0630 DL39 0.3g gbr/100g 2.88% ASTM D 1159 DL38 0.2g 6.43 gbr/100g 1.78% ASTM D 1159 DL38 8 SH/T 1551 SH/T 0630 ASTM D 1492 ASTM D 1159 GB

9 E P ph=8.2 / p H m L g g g...5

10 0.1mg/g(mL) 10mg/g(mL) % 100% 15.66% g 4 0 m L DL32 DL39 10

11 p H Seven - S e v e n p H I S F E T Seven SevenEasy SevenMulti - S e v e n M u l t i S e v e n E a s y SevenMulti SevenEasy ph p H RS232 I S F E T U S B T T L SevenEasy GLP S e v e n E a s y / / SevenMulti / W i n d o w s H y p e r - Terminal / / 11

12 METTLER TOLEDO GmbH, Analytical ( ) Sonnenbergstrasse 74 / CH-8603 Schwerzenbach, Switzerland Tel: Telefax: marketsupport.anachem@mt.com A. De Agostini P. Gilmer UserCom6 UserCom 7 - ( ) Mettler-Toledo Instruments (Shanghai) Ltd mtcs@public.sta.net.cn / / / / - DL5x ph ph DL31/ / 29 G DL5x DL32/ mtchina.com - * * - - ( ) 10/

2 Check - DE RE DR45 / RE40 SC1 /

2 Check - DE RE DR45 / RE40 SC1 / 11 - ph / - / - LabX P. Wyss - USP 1x10-5 g/cm -3 5 - DL50 Rondolino - 2 Check - DE RE DR45 / 1 2 3 4 1 5 6 RE40 SC1 / 7 9 1 2 8 S C 3 0 / DE RE 1 3 1 0 - S C 1 - D E 11 Incorrect > 25mPa s DR45 / 3 (1)