Water Determination in Paper with Potentiometric Method

Equipment

Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0338.100 double Pt electrode; input Pol

Reagents

HYDRANAL® Composite 5; D0

Sample

20 -30 mL methanol, conditioned to complete dryness
1.000 mL sample solution
extract app. 1.0g of paper (cut in small pieces) in 50 mL methanol (extraction medium)

Remarks

Calculations:

Water=(EP1-C38)*C39*C01/C00/C02;2;%

smpl size 0.02003 g
EP1 0.2260 ml
Water 5.29 %
Titer 5.0058 mg/ml
Blank 0.0145 ml
Water = content of water in paper in %
C00 = sample size / aliquot (1.0015 g / 50 mL = 0.02003 g/mL)
C01 = factor for % (0.1)
C02 = divisor (1)
C38 = blank value in mL of “Blank_KF“ method (0.0145 mL)
C39 = titer of HYDRANAL® Composite 5

Answer

Water = (0.2260-0.0145) x 5.0058 x 0.1 / 0.02003 / 1 = 5.29%

Mean from 3 determinations.
This method can be generally used for KF titrations with blank values.

· Adjust the calculation values C01 and C02 according the desired result unit and your sample size:

Unit RS Smpl size

Sample preparation:

Stir sample solution for app. ½ h to extract the water and take aliquots (see calculation).

Literature

Water determination by Karl Fisher titration, G. Wieland, GIT Verlag, Darmstadt (Germany)
HYDRANAL®, practical course, Water reagents according to Eugen Scholz, Riedel de Haën, Seelze (Germany)
Metrohm Application Bulletin No. 77: KF water determination

Blank Determination of Methanol with Potentiometric Method

Equipment
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0338.100 double Pt electrode; input Pol

Reagents
HYDRANAL® Composite 5; D0
Sample

20 -30 mL methanol, conditioned to complete dryness
1.000 mL methanol (extraction medium)

Remarks
Calculations:

Blank=EP1

Blank = blank of methanol (extraction medium)

Blank= 0.0145 mL

EP1 = 0.0145 mL

Common variables
C38 = MN1
Mean from 2-3 determinations.
This method can be generally used for KF blank determinations. For work with a KF Oven, you need an extraction time. Enter it in key , >titration parameters.

Use the same control parameters for the blank determination as for

the sample titrations.

For automatic curve output add in , >report “curve“.

Literature

Water determination by Karl Fisher titration, G. Wieland, GIT Verlag,Darmstadt (Germany)HYDRANAL®, practical course, Water reagents according to Eugen Scholz, Riedel de Haën, Seelze (Germany) Metrohm Application Bulletin No. 77: KF water determination

Method documentation

'pa
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:46 11
KFT Ipol Blank_KF
parameters
control parameters
EP at U 250 mV
dynamics 100 mV
max.rate max. ml/min
min.volume incr. min. ml
stop crit: drift
stop drift 20 ml/min
>titration parameters
titr.direction: -
pause 1 0 s
start V: OFF
pause 2 0 s
extr.time 0 s
dos.element: internal D0
I(pol) 50 mA
electrode test: OFF
temperature 25.0 °C
time interval 2 s
>stop conditions
stop V: abs.
stop V 99.99 ml
filling rate max. ml/min
>statistics
status: ON
mean n= 3
res.tab: original
>preselections

conditioning: ON
display drift: ON
drift corr: OFF
req.ident: OFF
req.smpl size: OFF
activate pulse: OFF
------------
'de
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:46
KFT Ipol Blank_KF
def
>formula

Blank=EP1

RS1 text Blank
RS1 decimal places 4
RS1 unit: ml
>silo calculations
match id: OFF
>common variables
C38=MN1
>report
report COM1:full;
>mean
MN1=RS1
>temporary variables
------------
'fr
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:45 11
KFT Ipol Blank_KF
EP1 0.0145 ml
Blank 0.0145 ml
mean( 2) +/-s s/%
Blank 0.0145 0.00000 ml 0.00
============
'cu
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:45 11
KFT IpolBlank_KF
2.0 s/div dV=0.05 ml/div
============
'st

751 GPD Titrino 15215 751.0010

date 97-03-12 time 10:46
statistics
## Blank
1 0.0145
2 0.0145
mean( 2) +/-s s/%
Blank 0.0145 0.00000 ml 0.00

Blank Determination of Methanol with Potentiometric Method

Equipment
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0338.100 double Pt electrode; input Pol

Reagents
HYDRANAL® Composite 5; D0
Sample

20 -30 mL methanol, conditioned to complete dryness
1.000 mL methanol (extraction medium)

Remarks
Calculations:

Blank=EP1

Blank = blank of methanol (extraction medium)

Blank= 0.0145 mL

EP1 = 0.0145 mL

Common variables
C38 = MN1
Mean from 2-3 determinations.
This method can be generally used for KF blank determinations. For work with a KF Oven, you need an extraction time. Enter it in key , >titration parameters.

Use the same control parameters for the blank determination as for

the sample titrations.

For automatic curve output add in , >report “curve“.

Literature

Water determination by Karl Fisher titration, G. Wieland, GIT Verlag,Darmstadt (Germany)HYDRANAL®, practical course, Water reagents according to Eugen Scholz, Riedel de Haën, Seelze (Germany) Metrohm Application Bulletin No. 77: KF water determination

Method documentation

'pa
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:46 11
KFT Ipol Blank_KF
parameters
control parameters
EP at U 250 mV
dynamics 100 mV
max.rate max. ml/min
min.volume incr. min. ml
stop crit: drift
stop drift 20 ml/min
>titration parameters
titr.direction: -
pause 1 0 s
start V: OFF
pause 2 0 s
extr.time 0 s
dos.element: internal D0
I(pol) 50 mA
electrode test: OFF
temperature 25.0 °C
time interval 2 s
>stop conditions
stop V: abs.
stop V 99.99 ml
filling rate max. ml/min
>statistics
status: ON
mean n= 3
res.tab: original
>preselections

conditioning: ON
display drift: ON
drift corr: OFF
req.ident: OFF
req.smpl size: OFF
activate pulse: OFF
------------
'de
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:46
KFT Ipol Blank_KF
def
>formula

Blank=EP1

RS1 text Blank
RS1 decimal places 4
RS1 unit: ml
>silo calculations
match id: OFF

>common variables

C38=MN1

>report

report COM1:full;

>mean

MN1=RS1

>temporary variables

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

'fr

751 GPD Titrino 15215 751.0010

date 97-03-12 time 10:45 11

KFT Ipol Blank_KF

EP1 0.0145 ml

Blank 0.0145 ml

mean( 2) +/-s s/%

Blank 0.0145 0.00000 ml 0.00

============

'cu

751 GPD Titrino 15215 751.0010

date 97-03-12 time 10:45 11

KFT IpolBlank_KF

2.0 s/div dV=0.05 ml/div

============

'st

751 GPD Titrino 15215 751.0010

date 97-03-12 time 10:46

statistics

## Blank

1 0.0145

2 0.0145

mean( 2) +/-s s/%

Blank 0.0145 0.00000 ml 0.00

Blank Determination of Methanol with Potentiometric Method

Equipment
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0338.100 double Pt electrode; input Pol

Reagents
HYDRANAL® Composite 5; D0
Sample

20 -30 mL methanol, conditioned to complete dryness
1.000 mL methanol (extraction medium)

Remarks
Calculations:

Blank=EP1

Blank = blank of methanol (extraction medium)

Blank= 0.0145 mL

EP1 = 0.0145 mL

Common variables
C38 = MN1
Mean from 2-3 determinations.
This method can be generally used for KF blank determinations. For work with a KF Oven, you need an extraction time. Enter it in key , >titration parameters.

Use the same control parameters for the blank determination as for

the sample titrations.

For automatic curve output add in , >report “curve“.

Literature

Water determination by Karl Fisher titration, G. Wieland, GIT Verlag,Darmstadt (Germany)HYDRANAL®, practical course, Water reagents according to Eugen Scholz, Riedel de Haën, Seelze (Germany) Metrohm Application Bulletin No. 77: KF water determination

Method documentation

'pa
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:46 11
KFT Ipol Blank_KF
parameters
control parameters
EP at U 250 mV
dynamics 100 mV
max.rate max. ml/min
min.volume incr. min. ml
stop crit: drift
stop drift 20 ml/min
>titration parameters
titr.direction: -
pause 1 0 s
start V: OFF
pause 2 0 s
extr.time 0 s
dos.element: internal D0
I(pol) 50 mA
electrode test: OFF
temperature 25.0 °C
time interval 2 s
>stop conditions
stop V: abs.
stop V 99.99 ml
filling rate max. ml/min
>statistics
status: ON
mean n= 3
res.tab: original
>preselections

conditioning: ON
display drift: ON
drift corr: OFF
req.ident: OFF
req.smpl size: OFF
activate pulse: OFF
------------
'de
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:46
KFT Ipol Blank_KF
def
>formula

Blank=EP1

RS1 text Blank
RS1 decimal places 4
RS1 unit: ml
>silo calculations
match id: OFF
>common variables
C38=MN1
>report
report COM1:full;
>mean
MN1=RS1
>temporary variables
------------
'fr
751 GPD Titrino 15215 751.0010
date 97-03-12 time 10:45 11
KFT Ipol Blank_KF

EP1 0.0145 ml

Blank 0.0145 ml

mean( 2) +/-s s/%

Blank 0.0145 0.00000 ml 0.00

============

'cu

751 GPD Titrino 15215 751.0010

date 97-03-12 time 10:45 11

KFT IpolBlank_KF

2.0 s/div dV=0.05 ml/div

============

'st

751 GPD Titrino 15215 751.0010

date 97-03-12 time 10:46

statistics

## Blank

1 0.0145

2 0.0145

mean( 2) +/-s s/%

Blank 0.0145 0.00000 ml 0.00

KF Titer Determination with Water by Potentiometric Method

KF Titer Determination with Water by Potentiometric Method

Equipment
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0338.100 double Pt electrode; input Pol

Reagents
HYDRANAL® Composite 5; D0

Sample
20 -30 mL methanol, conditioned to complete dryness
10 μL dist. water

Remarks
Calculations:

Titer=C00/EP1*C01;4;mg/ml

Titer = titer of HYDRANAL® Composite 5
C01 = factor (1000 if water is used as standard; if methanol is used, enter its water content in mg/mL)

Answer

Titer = 0.010 / 1.9975 x 1000 = 5.0063 mg/mL

EP1 = 1.9975 mL
C00 = 1000

Common variables
C39 = MN1
Mean from 5 determinations.
Water or methanol standard can be injected either with a microliter syringe or with any syringe and reweighed.
Adjust the calculation value C01 according to your sample size: water
C00 in g C01=1000
C00 in mL C01=Density of H2O [mg/mL] 1
Methanol standard
C00 in mL C01=Content of methanol [mg/mL]
C00 in mL C01=0.001 * content of methanol [mg/mL]
For automatic curve output add in , >report “curve“.

Literature
Water determination by Karl Fisher titration, G. Wieland, GIT Verlag, Darmstadt (Germany)
HYDRANAL®, practical course, Water reagents according to Eugen
Scholz, Riedel de Haën, Seelze (Germany)
Metrohm Application Bulletin No. 77: KF water determination

Method documentation

'pa
751 GPD Titrino 15215 751.0010
KFT Ipol H2OTiter
parameters
>control parameters
EP at U 250 mV
dynamics 100 mV
max.rate max. ml/min
min.volume incr. min. ml
stop crit: drift
stop drift 20 ml/min
>titration parameters
titr.direction: -
pause 1 0 s
start V: OFF
pause 2 0 s
extr.time 0 s
dos.element: internal D0
I(pol) 50 mA
electrode test: OFF
temperature 25.0 °C
time interval 2 s
>stop conditions
stop V: abs.
stop V 99.99 ml
filling rate max. ml/min
>statistics
status: ON
mean n= 5
res.tab: original
>preselections
conditioning: ON
display drift: ON
drift corr: OFF
req.ident: OFF
req.smpl size: value
activate pulse: OFF
------------
'fm
751 GPD Titrino 15215 751.0010
KFT Ipol H2OTiter
>calculations
Titer=C00/EP1*C01;4;mg/ml

C00= 0.010
C01= 1000
------------
'fr
751 GPD Titrino 15215 751.0010
KFT Ipol H2OTiter
smpl size 0.010 g
EP1 1.9975 ml
Titer 5.0063 mg/ml
mean( 5) +/-s s/%
Titer 5.0058 0.00287 mg/ml 0.06
============
'cu
751 GPD Titrino 15215 751.0010
KFT IpolH2OTiter
10.0 s/div dV=0.5 ml/div
============
'st
751 GPD Titrino 15215 751.0010
statistics
## Titer
1 5.0050
2 5.0075
3 5.0013
4 5.0088
5 5.0063
mean( 5) +/-s s/%
Titer 5.0058 0.00287 mg/ml 0.06

KF Titer Determination with Sodium Tartrat by Potentiometric Method

KF Titer Determination with Sodium Tartrate by Potentiometric Method

Equipment
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0338.100 double Pt electrode; input Pol

Reagents
HYDRANAL® Titrant 5; D0

Sample
20 -30 mL HYDRANAL® Solvent, conditioned to complete dryness app. 200 mg di-Sodium tartrate dihydrate
Water 15.66 ±0.05%

Remarks
Calculations:

Titer=C00/EP1*C01;4;mg/ml

Titer = titer of HYDRANAL® Titrant 5
C01 = water content * 10 (156,6)

Answer

Titer= 0.2294 / 7.508 x 156.6 = 4.7848 mg/mL

EP1 = 7.508 mL
C00 = 0.2294 g

Common variables
C39 = MN1
Mean from 5 determinations.
Reweigh the sodium tartrate in a weighing boat.
Adjust the calculation value C01 according to the unit of your sample
weight:

C00 in g C01=156.6
C00 in mg C01=0.1566
For automatic curve output add in , >report “curve“.

Literature
Water determination by Karl Fisher titration, G. Wieland, GIT Verlag,
Darmstadt (Germany)
HYDRANAL®, practical course, Water reagents according to Eugen
Scholz, Riedel de Haën, Seelze (Germany)
Metrohm Application Bulletin No. 77: KF water determination

Method documentation

'pa
751 GPD Titrino 15215 751.0010
KFT Ipol TarTiter
parameters
>control parameters
EP at U 250 mV
dynamics 100 mV
max.rate max. ml/min
min.volume incr. min. ml
stop crit: drift
stop drift 20 ml/min
>titration parameters
titr.direction: -
pause 1 0 s
start V: OFF
pause 2 0 s
extr.time 0 s
dos.element: internal D0
I(pol) 50 mA
electrode test: OFF
temperature 25.0 °C
time interval 2 s
>stop conditions
stop V: abs.
stop V 99.99 ml
filling rate max. ml/min
>statistics
status: ON
mean n= 5
res.tab: original
>preselections
conditioning: ON
display drift: ON
drift corr: OFF
req.ident: OFF
req.smpl size: value
activate pulse: OFF
------------
'fm
751 GPD Titrino 15215 751.0010
KFT Ipol TarTiter
>calculations

Titer=C00/EP1*C01;4;mg/ml

C00= 0.2294
C01= 156.6
------------
'fr
751 GPD Titrino 15215 751.0010
KFT Ipol TarTiter

smpl size 0.2294 g
EP1 7.508 ml
Titer 4.7848 mg/ml
mean( 5) +/-s s/%
Titer 4.7893 0.00506 mg/ml 0.11
============
'cu
751 GPD Titrino 15215 751.0010
KFT IpolTarTiter
20.0 s/div dV=2.0 ml/div
============
'st
751 GPD Titrino 15215 751.0010
statistics
## Titer
1 4.7936
2 4.7939
3 4.7830
4 4.7910
5 4.7848
mean( 5) +/-s s/%
Titer 4.7893 0.00506 mg/ml 0.11

Analysis of Spinning Bath with Potentiometric Method

Analysis of Spinning Bath With Potentiometric Method

Reagents
c(NaOH) = 0.1 mol/L; D0

Sample
0.1 mL c(ZnSO4) ≅ 0.1 mol/L in c(H2SO4) ≅ 1 mol/L
25 mL dist. water

Electrodes
6.0232.100 combined pH glass electrode; input 1

Remarks
• EP1: H₂SO₄ + 2OH^- ⇒ SO4 ^2- + 2H₂O

EP2: Zn²⁺ + 2 OH^- ⇒ Zn(OH)₂ (s)

Calculations:
H2SO4 = concentration of H2SO4 in g/L
ZnSO4 = concentration of ZnSO4 in g/L
C01 = concentration of titrating agent (0.1 mol/L)
C02 = molecular mass of H2SO4 (98.08 g/mol)
C03 = molecular mass of ZnSO4 (161.23 g/mol)
C04 = factor for “normality“ (2)
• For automatic curve output add in , >report “curve“.

Literature
Metrohm's Teachware on CD-ROM

Method documentation

'pa
751 GPD Titrino...15215...751.0010
SET pH...Spinning
parameters
>SET1
EP at pH...5.50
dynamics...3
max.rate ...5 ml/min
min.rate...1 μl/min
stop crit:...drift
stop drift ...20 μl/min
>SET2
EP at pH...9.50
dynamics...4
max.rate...1 ml/min
min.rate ...1 μl/min
stop crit:... drift
stop drift ... 20 μl/min
>titration parameters
titr.direction:...auto
pause 1... 0s
start V: ...OFF
pause 2...0s
extr.time... 0s
dos.element:...internal D0
meas.input:...1
temperature...25.0 °C
time interval...2s
>stop conditions
stop V:... abs.
stop V...99.99 ml
filling rate...max. ml/min
>statistics
status:...OFF
>preselections
conditioning:...OFF
req.ident:...OFF
req.smpl size:...OFF
activate pulse:...OFF
------------
'fm
751 GPD Titrino 15215 751.0010
SET pH...Spinning
>calculations

H₂SO₄=EP1*C01*C02/C04/C00;2;g/l
ZnSO₄=(EP2-EP1)*C01*C03/C04/C00;2;g/l

C00= 0.1
C01= 0.1
C02= 98.93
C03= 161.23
C04= 2
------------
'fr
751 GPD Titrino 15215 751.0010
pHc(init) 2.22 SET pH Spinning
smpl size 0.1 ml
EP1 2.011 ml 5.61
EP2 2.245 ml 9.53
H2SO4 99.47 g/l
ZnSO4 18.86 g/l
============
'cu
751 GPD Titrino 15215 751.0010
SET pH Spinning
20.0 s/div dV=0.5 ml/div