滴定における測定の不確かさMeasurement Uncertainty …

1 measurement Uncertainty MU .. 1 mol/l .. JIS A 5308 . a 1 mol l . mol l mol l . (JP). 4 3 3 . REAGENT CHEMICALS ninth edition ACS SPECIFICATIONS. Replication Duplicate standardizations for solutions from N to 1N should agree at least to within 2 parts in 1000. Duplicates for N. solutions may differ by as much as 10 parts in 1000. If deviations are greater than indicated, the determinations should be repeated until the criteria are met. Degree of rigour a. consider the requirements and limitations of the test method and the need to comply with good practice in the particular sector.. O O. H NaOH H. N S OH N S ONa H2 O.

2 H H. O O. (JIS K 8005). kPa 48 .. g 1000 M P . c( NaOH ) =. F V. 25 ml . c (NaOH) : (mol/l). 1000 :ml l . M : (g) . ml . : (g/mol). : . : (ml) .. 1 M Sodium hydroxide Titrate ml of the sodium hydroxide solution with 1 M hydrochloric acid using the indicator prescribed in the assay in which 1 M sodium hydroxide is used. The solution complies with the following test. Titrate ml of hydrochloric acid of the same molarity with the solution of sodium hydroxide, using ml of phenol phthalein solution R as indicator. European Pharmacopeia 4th Edition 2002 . NORMAL ALKALI HYDROXIDE. Method I-Accurately measure from a burette 30-40 ml of 1 N hydrochloric or sulfuric acid into a flask, and dilute with 50 ml of carbon dioxide- free water.

3 Add 3 drops of phenolphthalein and titrate with the sodium hydroxide from a burette to the production of a slight but permanent pink color. REAGENT CHEMICALS and STANDARDS .. (ml) .. 1 mol/lNaOH 25 ml 1 mol/l HCl 1 mol/lNaOH Lot. 509F9110 1 mol/l HCl Lot. 509F9203 . 1 mol/lHCl .. ( , , , .. Identifying the components of Uncertainty The laboratory should identify all the significant components of Uncertainty for each test. Components contributing less than 1/5 to 1/3 of the total measurement Uncertainty will not usually have much impact on the total measurement Uncertainty . Even where reliance is to be made on overall precision data or where note 2 of clause of ISO/IEC 17025 is to apply, the laboratory should at least attempt to identify all significant components.)

4 A B .. IUPAC .. 80 g10 .. 2 .. 10 . pH .. 25 ml10 .. ( ) 3 .. u (P ) = = 3.. IUPAC HOSO2 NH2 . IUPAC 3 .. 94 07 040 3 94 82 12. 4 3 17 3 4 2 51. 7 2 12 1 7 67 12. 9 1 9.. F = 3 . 02382 + 47 . 9982 + 14 . 0067 + 32 . 065 = 97 .09372 g / mol u( ). u( F ) = 0 .00012 2 + 0 .00051 2 + 0 . 00012 2 + 0 . 0029 2 = 0 . 0029 g / mol . ppm .. n=1 n=2 n=3 . 3 JIS K 8001-1985 . pH pH 3 . H H . 0 30 60 90 120 150 180 210 240.. 2 JIS Z 8703 1 JIS R 3505. 10 2 /h . 2003 2 . JIS Z 8703 (ISO 554 IEC 160) . 20 23 25 27 (2 ). 26. 50 65 . 25. 24. 23. 22. 2 2 21. 20. 5 5 1 1 19. 18. 10 10 5 5 17. 20 20 15 15 16. 15. 5:40'08". 6:38'08".

5 7:36'08". 8:34'08". 9:32'08". 0:02'08". 1:00'08". 1:58'08". 2:56'08". 3:54'08". 4:52'08". 10:30'08". 11:28'08". 12:26'08". 13:24'08". 14:22'08". 15:20'08". 16:18'08". 17:16'08". 18:14'08". 19:12'08". 20:10'08". 21:08'08". 22:06'08". 23:04'08".. 1 mol/lNaOH . 12 .. 20 10 40 . 6 12 5 n=3 0 6 12.. F .. 208G6037 mol/ 208G6001 207G9182 mol/ 208G9064 p= ) Uncertainty arising from sampling : Where sampling (or sub- sampling ) is to be treated as part of the test, the Uncertainty arising from such sampling shall be considered by the laboratory.. mg( 15g) . 15 g 077 2 2 . g g g . 1 6 4 8. 2 6 4 8. 3 6 5 9. 10 . 4 5 4 9.. 5 7 5 8.

6 A B C 6 5 5 0. 9 9 9 7 5 4 9. 048 074 085 8 5 4 9. 9 5 5 0.. 10 6 5 9. u ( M ) = 2 + 2 2. = g 9. 074.. 0-25ml 10 .. A B C. ml 0 6 5. 0 25 ml .. 23 3 10 95 JIS . 1 . mol/l . Vt 20 V20 (ml) (ml). d . V t =V 20 [1 + (t 20 )] 1 . t ( 010 K-1 ). d 20 (g/ml). 20 20 (g/ml). ( ).. g 250 ml 10 ml . A B C. 1 . 2 . 3 . 4 . 5 . 6 . 7 . 8 . 9 . 10 . SD 22 83 68.. 90%~99% . 40 25 ml .. y = x - 2. R = .. 100g mg 25 35 45 55 65 75 25ml 25ml (s). 25ml 25ml g 0 .000024 2 + 2 + 2 + 2 + 2 = . u (V ) = 0 . 0076 2. + 0 . 00030 2. + 0 . 00568 2. = 0 . 00949.. X . M 5 g 138 g 055. 1 058 058. 72 g/mol 9 g/mol 030. ml 49 ml 367. 1000 C NaOH = = mol / l 97.

7 09372 u(C NaOH ). = 2 + 2 + 2 + 2 = CNaOH. u (C NaOH ) = = mol / l n=10 n 1= 9 95% t .. U = 0 .00038 = / l.