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Supplement I to the Japanese Pharmacopoeia Fourteenth Edition

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1374 General Tests, Processes and Apparatus<br />

<strong>Supplement</strong> I, JP XIV<br />

contained in <strong>the</strong> apparatus.<br />

Conductivity measurement is generally performed by using<br />

an immersion-type cell. A pair of platinum electrodes,<br />

<strong>the</strong> surfaces of which are coated with platinum black, is ˆxed<br />

in parallel. Both electrodes are generally protected by a glass<br />

tube <strong>to</strong> prevent physical shocks.<br />

When <strong>the</strong> surface area of <strong>the</strong> electrode is A (cm 2 ), and <strong>the</strong><br />

separation distance of <strong>the</strong> two electrodes is l (cm), <strong>the</strong> cell<br />

constant C (cm -1 ) is given by <strong>the</strong> following equation.<br />

C = a・(l/A )<br />

a is a dimensionless numerical coe‹cient, and it is characteristic<br />

of <strong>the</strong> cell design.<br />

In addition <strong>to</strong> <strong>the</strong> immersion-type cell, <strong>the</strong>re are ‰owthrough-type<br />

and insert-in-pipe-type cells. These cells are set<br />

or inserted in an appropriate position in <strong>the</strong> ‰ow system for<br />

moni<strong>to</strong>ring <strong>the</strong> quality of water continuously or intermittently,<br />

during <strong>the</strong> preparation of highly puriˆed water.<br />

Standard Solution of Potassium Chloride<br />

After pulverizing an appropriate amount of potassium<br />

chloride for conductivity measurement, dry it at 500 – 6009C<br />

for 4 hours. Take an indicated amount of <strong>the</strong> dried potassium<br />

chloride, as shown in Table 1, dissolve it in distilled or<br />

puriˆed water (conductivity less than 2 mS・cm -1 ), previously<br />

boiled and cooled, and adjust <strong>to</strong> make 1000.0 g, for<br />

preparation of <strong>the</strong> standard solutions. The conductivity and<br />

<strong>the</strong> resistivity of <strong>the</strong> respective standard solutions at 209C<br />

are indicated in Table 1. These standard solutions should be<br />

kept in tightly closed polyethylene or hard glass bottles.<br />

Table 1. Conductivity and Resistivity of <strong>the</strong> Standard<br />

Solutions of Potassium Chloride at 209C<br />

Concentration<br />

(g/1000.0 g)<br />

Conductivity k<br />

(mS・cm -1 )<br />

Resistivity r<br />

(Q・cm)<br />

0.7455 1330 752<br />

0.0746 133.0 7519<br />

0.0149 26.6 37594<br />

When measurement at 209C cannotbedone,<strong>the</strong>indicated<br />

value of conductivity for <strong>the</strong> respective standard solution<br />

(Table 1), can be corrected by using <strong>the</strong> equation below.<br />

However, <strong>the</strong> equation is valid only within <strong>the</strong> range of 20 ±<br />

59C.<br />

k T = k 20 [1 + 0.021(T - 20)]<br />

T: Measuring temperature speciˆed in <strong>the</strong> monograph<br />

k T : Calculated conductivity of <strong>the</strong> KCl standard solution<br />

at T9C<br />

k 20 : Conductivity of <strong>the</strong> KCl standard solution at 209C<br />

Operating Procedure<br />

(1) Cell Constant<br />

An appropriate conductivity cell should be chosen according<br />

<strong>to</strong> <strong>the</strong> expected conductivity of <strong>the</strong> sample solution. The<br />

higher <strong>the</strong> expected conductivity, <strong>the</strong> larger <strong>the</strong> cell constant<br />

required for <strong>the</strong> conductivity cell, so that <strong>the</strong> electrical<br />

resistance is within <strong>the</strong> measuring range of <strong>the</strong> apparatus<br />

being used. Conductivity cells with a cell constant of <strong>the</strong> order<br />

of 0.1 cm -1 ,1cm -1 ,or10cm -1 , are generally used.<br />

For determination or conˆrmation of <strong>the</strong> cell constant, an<br />

appropriate KCl standard solution should be chosen and<br />

prepared, taking account of <strong>the</strong> expected conductivity of <strong>the</strong><br />

sample solution <strong>to</strong> be measured. Rinse <strong>the</strong> cell several times<br />

with distilled water. Next, after rinsing <strong>the</strong> cell 2 – 3 times<br />

with<strong>the</strong>standardsolutionusedfor<strong>the</strong>cellconstantdetermination,<br />

immerse <strong>the</strong> cell in <strong>the</strong> standard solution contained<br />

in a measuring vessel. After conˆrming that <strong>the</strong> temperature<br />

of <strong>the</strong> standard solution is maintained at 20 ± 0.19C orat<br />

<strong>the</strong> temperature speciˆed in <strong>the</strong> monograph, measure <strong>the</strong><br />

resistance R KCl or <strong>the</strong> conductance G KCl of <strong>the</strong> standard solution,<br />

and calculate <strong>the</strong> cell constant C (cm -1 )byuseof<strong>the</strong><br />

following equation.<br />

C = R KCl ・k KCl or C = k KCl /G KCl<br />

R KCl : Measured resistance (MQ)<br />

G KCl : Measured conductance (mS)<br />

k KCl : Conductivity of <strong>the</strong> standard solution being used<br />

(mS・cm -1 )<br />

The measured cell constant should be consistent with <strong>the</strong><br />

given value within 5z. Ifitisnotconsistent,coat<strong>the</strong>electrodes<br />

with platinum black again, or replace <strong>the</strong> cell with a<br />

new one.<br />

(2) Suitability Test for <strong>the</strong> Apparatus<br />

Using an appropriate KCl standard solution according <strong>to</strong><br />

<strong>the</strong> expected conductivity of <strong>the</strong> sample solution, perform<br />

<strong>the</strong> suitability test for <strong>the</strong> apparatus. Rinse <strong>the</strong> conductivity<br />

cell several times with distilled water, and rinse again 2 – 3<br />

times with <strong>the</strong> selected standard solution. Fill <strong>the</strong> standard<br />

solution in <strong>the</strong> measuring vessel. After conˆrming that <strong>the</strong><br />

temperature of <strong>the</strong> measuring system is maintained at 20 ±<br />

0.19C, measure <strong>the</strong> conductivity of <strong>the</strong> standard solution.<br />

When this measuring procedure is repeated several times, <strong>the</strong><br />

average conductivity should be consistent with an indicated<br />

value in Table 1 within 5z. Fur<strong>the</strong>r, <strong>the</strong> relative standard<br />

deviation should be less than 2z.<br />

(3) Measurement<br />

After conˆrmation of <strong>the</strong> suitability of <strong>the</strong> apparatus, perform<br />

<strong>the</strong> conductivity measurement for <strong>the</strong> sample solution.<br />

Unless o<strong>the</strong>rwise speciˆed, <strong>the</strong> preparation method for sample<br />

solution should be as speciˆed in <strong>the</strong> respective monograph.<br />

Rinse <strong>the</strong> conductivity cell several times with distilled<br />

water, and rinse again 2 – 3 times with sample solution. Immerse<br />

<strong>the</strong> cell in <strong>the</strong> sample solution placed in a measuring<br />

vessel. If necessary, agitate gently <strong>the</strong> sample solution. After<br />

conˆrming that <strong>the</strong> temperature of <strong>the</strong> sample solution is<br />

maintained at 20 ± 0.19C or at <strong>the</strong> temperature speciˆed in<br />

<strong>the</strong> monograph, measure <strong>the</strong> resistance R T (MQ) or conductance<br />

G T (mS) of <strong>the</strong> sample solution, and calculate <strong>the</strong> conductivity<br />

k T by using <strong>the</strong> following equation.<br />

k T = CG T or k T = C/R T<br />

Items such as <strong>the</strong> sample preparation method, <strong>the</strong> necessity<br />

of blank correction, <strong>the</strong> calculation method, <strong>the</strong> speciˆcation<br />

value, and <strong>the</strong> measuring temperature should be described<br />

in <strong>the</strong> monograph, if necessary.

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