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1、STD-JIS K OLL3-ENGL 3997 4933608 0549526 202 M J IS JAPANESE I NDUSTRIAL STANDARD Translated and Published by Japanese Standards Association General rules for methods of potentiometric, amperometric, coulometric, and Karl-Fischer tit rat ions ICs 71.040.40 Descriptors : potentiometric methods, amper
2、ometric methods, coulometric methods, electro-analytical methods, instrumental methods of analysis Reference number : JIS K 0113 : 1997 (E) 13 S Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2
3、007 19:54:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS K 0113-ENGL 1997 m 4733608 0549527 149 m K 0113: 1997 This translation has been made based on the original Japanese Industrial Standard revised by the Minister of International Trade and Industry through d
4、eliberations at Japanese Industrial Standards Committee in accordance with the Industrial Standardization Law: Date of Establishment: 1962-05-01 Date of Revision: 1997-09-20 Date of Public Notice in Official Gazette: 1997-09-22 Investigated by: Japanese Industrial Standards Committee Divisional Coun
5、cil on Basic Items JIS K 0113: 1997, First English edition published in 1998-03 Translated and published by: Japanese Standards Association 4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN In the event of any doubts arising as to the contents, the original JIS is to be the final authority. O JSA 19
6、98 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in Japan Copyright Japanese Standards A
7、ssociation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:54:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD=JIS K OLL3-ENGL 1997 4733608 0549528 085 JAPANESE INDUSTRIAL STANDARD JIS K 0113 : 1
8、997 General rules for methods of potentiometric, amperometric, coulometric, and Karl-Fischer titrations 1 Scope This Japanese Industrial Standard specifies general rules applicable when quanti- tative analysis is carried out according to potentiometric, amperometric, coulometric, or Karl-Fischer tit
9、ration. i Remarks 1 The normative references to this Standard are as follows. JIS K 0050 JIS K 0126 JIS K 0211 JIS K 0213 JIS K 8322 JIS K 8540 JIS K 8574 JIS K 8777 JIS K 8891 JIS K 8895 JIS K 8920 General rules for chemical analysis General rules for flow injection analysis Technical terms for ana
10、lytical chemistry (general part) Technical terms for analytical chemistry (electrochemistry division) Chloroform Sodium (+)-tartrate dihydrate Potassium hydroxide Pyridine Methanol 2-methoxyethanol Iodine 2 The International Standard corresponding to this Standard is as follows. IS0 760-1978 Determi
11、nation of water - Karl Fischer method (General method) Informative reference: In IS0 760 in which Karl-Fischer titration has been specified, in order to detect the end point of titration, two methods are specified, one is method by visual titration, and the other is electrically detecting method, ho
12、wever, the latter is recommended because of its accuracy for measurement, therefore in this Standard the elctrically detecting method only is specified. 2 Matters in common Matters in common shall follow JIS K 0050. 3 JIS K 0211 and JIS K 0213, and for others the following definitions apply. Definit
13、ions For the purpose of this Standard, main definitions are in accordance with (1) titration curve The curve expressing the state of progression of titration, for the purpose of deciding the end point of titration, in which any of indicator potential difference, pH, or indicator electric current (Y)
14、 is graduated on the ordinate axis, and either the volume of titrant needed for titration or the quantity of electricity (X) needed for generation of titration agent is graduated on the abscissa axis. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employe
15、es/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:54:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS K O113-ENGL 1997 4933608 0549529 T 1 1 2 K 0113 : 1997 (2) differential titration curve The curve plotted by graduating either difference quantity (A
16、Y/AX) or differential quantity (dY/dX) of the titration curve on the ordinate axis and graduating the value of X on the abscissa axis. (3) indicator electrode An electrode for measuring either the electric potential or current that is used for determining the end point of titration. (4) indicator po
17、tential difference The electric potential difference of indicator electrode measured to the reference electrode. (5) indicator current The electric current flowing through indicator electrode. (6) variation rate of potential difference The value of OY/OX or dY/dX when the potential difference is den
18、oted Y. (7) solution to be titrated A solution to be titrated for carrying out the determination of objective component. (8) titrant A solution containing the titration agent of known concentration. (9) water reference solution The solution in which the mass concentration of water is known. 4 shall
19、be classified as follows. Classification of analysis methods The analysis methods specified in this Standard (1) Potentiometric titration method (2) Amperometric titration method (3) The titration method which uses indicator potential The titration method which uses indicator current difference for
20、detection of end point. for detection of end point. Coulometric titration method The titration method in which titration agent is elec- trolytically generated and the amount of objective component is obtained from the quantity of electricity required for its generation. (4) Karl-Fischer titration me
21、thod The titration method to obtain water content making use of Karl-Fischer reagent. Remarks : Potentiometric titration method and amperometric titration method are both named based on the physical quantity employed for the end-point detection, therefore they may overlap with coulometric titration
22、method. 5 Potentiometric titration method 5.1 Apparatus 5.1.1 part, control part, and display-recording part. Its example is shown in Fig. 1. Configuration The potentiometric titration apparatus is composed of, a titration Copyright Japanese Standards Association Provided by IHS under license with J
23、SALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:54:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD.JIS K 0113-ENGL 1997 4933608 0549530 733 - 3 KO113 : 1997 Display- recording Part Titration part I Titration vessel Indicator Y Ref
24、erence electrode Control Part Fig. 1 Configuration of potentiometric titration apparatus (example) 5.1.2 Titration part Titration part is composed of, a titration vessel, detector, and titration agent adding apparatus. (i) Titration vessel The titration vessel is a vessel for titration, and is capab
25、le of being equipped with a detector and titration agent adding apparatus, and of agitating the solution. The material of the vessel shall be resistant against dissolving and deteri- oration. (2) Detector The detector is composed of an indicator electrode and reference electrode. (3) Titration agent
26、 adding apparatus The titration agent adding apparatus is an appa- ratus for quantitatively adding of titrant () when titration solution is used, and it shall be as specified in 7.1.2 (3) when coulometric titration is used. Note ( I ) For instance, a buret or automatic buret. 5.1.3 Control part The
27、control part shall have performances to amplify indicator electric potential difference by means of an amplifier with high input resistance, and to transduce it into the signal by which the display-recording part and titration agent adding apparatus are operated. 5.1.4 Display-recording part The dis
28、play-recording part shall have performances to display or record the indicator electric potential difference. As occasion demands, the device to display or record titration curve, titration results, etc. is attached. Remarks: A pH meter may be used in place of a control part and display-recording pa
29、rt. 5.2 Procedures 5.2.1 Prepare the titration curve or differential titration curve by plotting the indicator potential difference () or pH on Y axis and the volume of titrant on X axis. Carefully plot the curve to make the curve near its end point clear. In the case of coulometric titration, the q
30、uantity of electricity fed into Preparation of titration curve or differential titration curve Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:54:59 MDTNo reproduction or networking perm
31、itted without license from IHS -,-,- STD-JIS K OLL3-ENGL 1777 4733b08 0547531 b7T 4 K 0113 : 1997 titration agent adding apparatus or the volume of titration agent calculated from it shall be plotted on X axis. Note ( 2 ) The absolute value may be employed as Y, if any confusion is not antici- pated
32、. 5.2.2 Determination of end point The determination of end point shall be as follows : (1) When the titration curve is used, either of next two methods shall be used. (a) Inflection-point method When the inflection point of or the maximum inclination point of the titration curve is found with neces
33、sary accuracy, take the reading on abscissa as the end point. As shown in Fig. 2, draw two lines, with 45 o gradient, tangential to the titration curve, draw another line which is equidistant and parallel to these two lines, and read the intersecting point of the titration curve and this line on abs
34、cissa as the end point. When employing differential titration curve, read the point where the absolute value of variation rate of potential difference shows the maximum value on the abscissa, to find the end point. (b) Intersecting-point method (2) I End point Volume of titrant added Fig. 2 Determin
35、ation of end point (example) 5.2.3 Manual titration (1) The preparation of titration curve shall follow 5.2.1. (2) The determination of end point shall follow 5.2.2. (3) Other procedures than above shall comply with JIS K 0050 as appropriate. 5.2.4 Automatic titration Among automatic titration, ther
36、e are the titration by automatic end-point detecting type, titration by end-point potential setting type, and titration by titration-curve automatic recording type. (1) Titration by automatic end-point detecting type Detect the point where the varia- tion rate of potential difference becomes the max
37、imum, make it the end point, and express or record any one of the volume of titrant, or the quantity of electricity supplied to the titration agent adding apparatus, or the results obtained by operational treatment of them. Copyright Japanese Standards Association Provided by IHS under license with
38、JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:54:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS K OLL3-ENGL 1997 m 4933b08 0549532 506 m 5 K 0113 : 1997 (2) Titration by end-point potential setting type Make the instant wh
39、en indicator potential difference has reached the preliminarily set value as the end point, and express or record any one of the volume of titrant, or the quantity of electricity supplied to the titration agent adding apparatus, or the results obtained by operational treatment of them. (3) Titration
40、 by titration-curve automatic recording type differential titration curve. The way to determine the end point shall follow 5.2.2. Record the titration curve or 5.3 Arrangement of record When potentiometric titration is carried out, the items, which are thought to be necessary among the following ite
41、ms, shall be arranged and recorded. In the case of coulometric titration, however, it shall be as stated in 7 . 3 . Date and name of measurer Manufacturers name and type code of potentiometric titration apparatus. In the case where accessaries are used, their names and types. Preparation method of s
42、olution to be titrated Composition and standardization method of titrant Type and specification of indicator electrode and reference electrode Titration conditions (temperature, condition for agitating, titration rate, existence of inert-gas ventilation, or others) Volume of titrant required until e
43、nd point, and indicator potential difference or pH value at end point (or the preliminarily set indicator potential difference or pH value in the case of automatic titration of end-point potential setting type) Results of titration Other matters 5.4 Maintenance and control 5.4.1 Installation of pote
44、ntiometric titration apparatus The potentiometric titration apparatus shall be installed at a place complying with the following requirements: (1) The atmosphere shall be at a temperature 5 O C to 35 O C , a relative humidity not exceed- ing 85 % and shall not fluctuate rapidly. (2) There shall be n
45、o vibration, nor water leakage, nor direct sunshine. (3) Corrosive gas and dust shall be little and the ventilation shall be good. (4) There shall be no electrical noise which may cause interference. 5.4.2 Precautions for safety (1) ( 2 ) All electrical wirings shall be electrically safe, and their
46、insulation and earthing shall be securely executed. The sample and reagents shall be handled carefully by taking their explosiveness, inflammability, poisonousness and deleteriousness sufficiently into consideration. When discarding them, they shall be stabilized and made innocuous. Copyright Japane
47、se Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:54:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS K 0113-ENGL 1997 = 4933608 0549533 442 6 K 0113 : 1997 5.5 Matters
48、 to be described on detail specification At specifying the analysis method by potentiometric titration method, at least the following items shall be specified. However, in the case of coulometric titration method, the matters shall be as specified in 7.5. Objective component at measuring and its concentration range Sampling method and preservation method of sample Preparation method of solution to be titrated Components, concentration range, and standardization method of titrant Type and specification of indicator electrode and reference electrode Determination method for end point