6 "diazo – Metrohm 794 Basic Titrino User Manual

Page 174

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6.3. User methods

794 Basic Titrino

170

6.3.6 "Diazo"

Diazotation of sulfonamides and primary

amines.

Electrode:

6.0341.100 Pt-Titrode, at measuring input 1

Titrant:

c(NaNO

2

) = 0.1 mol/L.

Solvent:

w(HBr) = 0.3 (30%)

Sample:

Dilute 0.2 – 0.5 mmol of the substance to be

determined in 30 mL solvent and add 20 mL

dist. water. Titrate immediately.

– Sample size in g

– Molar mass of the substance to be determined

– Normality of the titrant (0.1*titer)

– Factor for %

'pa

794 Titrino 01102 794.0010

date 2002-01-03 time 09:43 0

MET U Diazo

parameters

>titration parameters

V step 0.10 ml

titr.rate max. ml/min

signal drift OFF mV/min

equilibr.time 20 s

start V: abs.

start V 0.5 ml

dos.rate max. ml/min

pause 80 s

meas.input: 1

temperature 25.0 °C

>stop conditions

stop V: abs.

stop V 6.00 ml

stop U OFF mV

stop EP 9

filling rate max. ml/min

>statistics

status: OFF

>evaluation

EPC 30 mV

EP recognition: greatest

fix EP1 at U OFF mV

pK/HNP: OFF

>preselections

req.ident: OFF

req.smpl size: value

activate pulse: OFF

------------

'fm

794 Titrino 01102 794.0010

date 2002-01-03 time 09:43 0

MET U Diazo

>calculations

Content=EP1*C01*C02*C03/C00;2;%

C00= 1.0

C01= 1

C02= 1

C03= 0.1

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