METTLER TOLEDO Application M007

Titer Determination of EDTA 0.1 mol/L with Zinc Sulfate

Titer determination of EDTA by complexometric titration at pH 10 with zinc sulfate as a standard,
TM
Eriochrome Black T as color indicator and DP5 Phototrode (660 nm) as a photometric sensor.

Sample Zinc sulphate solution, ZnSO4 Preparation and Procedures

c(ZnSO4) = 0.1 mol/L
CAUTION
5.0 mL
‐ Use safety goggles, a lab coat and wear gloves.
Work in a fume hood.
Compound Zinc sulfate , ZnSO4 ‐ Ensure accurate cleaning of sensor is sufficient
M = 161.44, z = 1 after each titration.
Sample titration :
Chemicals ‐ 40 mL deionized water
‐ 10 mL Ammonia Buffer pH 10 ‐ Dispense 5 mL 0.1 mol/L ZnSO4 solution in a
‐ Indicator: titration beaker.
0.1 mL (≈3 drops) of 0.1% Erio T ‐ Add 0.1-0.2 mL of Eriochrome Black T
(in ethanol)
‐ Start method
‐ Ethanol
‐ 10 mL Ammonia Buffer pH 10 is added from the
Titrant Ethylenediaminetetraacetic acid peristaltic pump.
disodium, EDTA-Na2
‐ 40 mL deionized water is added from the
C10H14N22Na2O8 x 2 H2O
membrane pump.
c(EDTA-Na2) = 0.1 mol/L ‐ After stirring, titration is started
‐ Color change observed: red to violet.
Standard -- ‐ After completion of each sample, sensor, stirrer
and titration tubes will be rinsed by deionized
TM water by means of membrane pump.
Indication DP5 Phototrode (660 nm)
(color change: red-violet) ‐ Subsequently, the sensor is cleaned in ethanol
in the conditioning beaker placed on the sample
Chemistry EDTA-Na2 + Zn
2+
 changer rack.
+
EDTA-Zn + 2 Na
Remarks
Calculation R= m/(VEQ*c*C)
‐ Prior to use, adjust the output signal of the DP5
C= 1/(cst*z)
to approx. 1000 mV in deionized water by
turning the small knob on the housing.
VEQ = Titrant consumption (mL)
c= Titrant concentration (mol/L) ‐ Rinsing and conditioning of the photometric
cst = Concentration standard sensor is crucial to achieve accurate and precise
solution (mol/L) results.
cst = 0.1 mol/L
m = Sample size (mL) ‐ Rinse the photometric sensor with ethanol to
M = Sample molar mass (g/mol) remove adherent material sticking on its mirror.
z= Sample equivalent number
‐ Avoid formation of bubbles during titration by
keeping low speed rate of stirrer, as they disturb
the photometric indication.
Waste Zinc is precipitated with NaOH
disposal or Ca(OH)2 and then filtered. ‐ This method allows a fully automated analysis
Precipitate is classified as procedure. The method can be modified for
special waste; the solution is manual operation. Select “Manual stand” in the
neutralized before final disposal method function “Titration stand”.
Author, Geeta Naik, IMSG
Version 2.0
Version Revised: C. De Caro, MSG AnaChem

METTLER TOLEDO Page 1 of 4 Titration Application M007

 Instruments ‐ Titration Excellence T50/T70/T90
(Other Titrators: with modification or manual operation are necessary)
‐ Rondo 20 Sample Changer with Power shower™ (ME- 51108003)
‐ 1 x SP250 Peristaltic pump
‐ XP205 Balance

Accessories ‐ PP Titration beakers (ME- 00101974)

®
‐ LabX pro titration software

Results
All results
Method-ID STDEDTA
Sample ZnSO4 (1/6)
R1 (1/6) 0.99367
Sample ZnSO4 (2/6)
R1 (2/6) 0.99217
Sample ZnSO4 (3/6)
R1 (3/6) 0.99255
Sample ZnSO4 (4/6)
R1 (4/6) 0.99235
Sample ZnSO4 (5/6)
R1 (5/6) 0.99225
Sample ZnSO4 (6/6)
R1 (6/6) 0.99215

Statistics
Method-ID STDEDTA
R1 0.99252
Samples 6
Mean 0.993
s 0.00058
srel 0.058%

Titration curve

METTLER TOLEDO Page 2 of 4 Titration Application M007

 Table of measured values
Volume Increment Signal Change 1st deriv. Time Temperature
mL mL mV mV mV/mL s °C
0.0000 NaN 606.3 NaN NaN 0 25.0
0.0100 0.0100 614.5 8.2 NaN 16 25.0
…. …. …. …. …. …. ….
4.9990 0.0100 569.7 -18.9 -2155.81 391 25.0
5.0090 0.0100 543.7 -26.0 -4169.69 397 25.0
5.0190 0.0100 504.2 -39.5 -6796.49 404 25.0
5.0290 0.0100 439.6 -64.6 -8851.89 410 25.0
5.0390 0.0100 327.2 -112.4 -9016.68 417 25.0
EQP1 5.039443 NaN 321.3 NaN -9016.68 NaN 25.0
5.0490 0.0100 194.3 -132.9 -6428.85 423 25.0
5.0590 0.0100 124.3 -70.0 -4849.34 429 25.0
5.0690 0.0100 102.3 -22.0 -4395.62 435 25.0
5.0790 0.0100 94.0 -8.3 -3093.49 442 25.0
5.0980 0.0190 87.6 -6.4 -1430.45 448 25.0
5.1430 0.0450 83.0 -4.6 -381.31 454 25.0
5.2430 0.1000 80.7 -2.3 -56.93 460 25.0
5.3430 0.1000 80.0 -0.7 -9.10 466 25.0
5.4430 0.1000 79.8 -0.2 1.26 472 25.0
5.5430 0.1000 79.8 0.0 3.06 478 25.0
5.6430 0.1000 80.0 0.2 2.70 484 25.0
5.7430 0.1000 80.2 0.2 2.47 490 25.0
5.8430 0.1000 80.4 0.2 2.54 496 25.0
5.9430 0.1000 80.7 0.3 2.62 502 25.0
6.0430 0.1000 80.9 0.2 2.70 508 25.0
6.1430 0.1000 81.2 0.3 2.86 514 25.0
6.2430 0.1000 81.5 0.3 2.90 521 25.0
6.3430 0.1000 81.8 0.3 3.06 527 25.0
6.4430 0.1000 82.1 0.3 3.10 533 25.0
6.5430 0.1000 82.4 0.3 3.07 539 25.0
6.6430 0.1000 82.7 0.3 NaN 545 25.0
6.7430 0.1000 83.1 0.4 NaN 551 25.0
6.8430 0.1000 83.3 0.2 NaN 557 25.0
6.9430 0.1000 83.7 0.4 NaN 563 25.0
7.0000 0.0570 83.9 0.2 NaN 569 25.0

Comments

• Eriochrome Black T indicator solution:

Weigh 0.5 g of Eriochrome Black T in 100 mL volumetric flask, dissolve and make up the volume with
95% ethanol.

• Ammonia buffer pH 10:

Weigh 6.4 g of ammonium chloride in 100 mL volumetric flask, dissolve in 60 mL ammonia, and
make up the volume with deionized water.

METTLER TOLEDO Page 3 of 4 Titration Application M007

 Method

001 Title 008 Calculation R1

Type Titer determination Result Titer
Compatible with T50 / T70 / T90 Result unit --
ID STDEDTA Formula R1=m/(VEQ*c*C)
Title Titer with EQP Constant C=1/(cst*z)
Author admin M M[None]
Date/Time . . . z z[None]
Modified on . . . Decimal places 5
Modified by admin Result limits No
Protect No Record statistics Yes
SOP None Extra statistical func. No
Send to buffer No
002 Sample (Titer) Condition No
Titrant EDTA
Concentration 0.1[mol/L] 009 Rinse
Standard Zinc sulphate Auxiliary reagent Water
Type of standard liquid Rinse cycles 1
Entry type Fixed volume Vol. per cycles 15 mL
Volume 5 mL Position Current position
Correction factor 1.0 Drain No
Temperature 25.0°C Condition No

003 Titration stand (Rondo/Tower A) 010 Conditioning

Type Rondo/Tower A Type Fix
Titration stand Rondo60/1A Interval 1
Lid handling No Position Conditioning beaker
Time 30 s
004 Pump Speed 10 %
Auxiliary reagent Buffer pH10 Condition No
Volume 10 mL
Condition No 011 End of sample

005 Pump 012 Titer

Auxiliary reagent Water Titrant EDTA
Volume 40 mL Concentration 0.1 mol/L
Condition No TITER Mean [R1]
Limits No
006 Stir Condition No
Speed 10 %
Duration 30 s 013 Calculation R2
Condition No Result Mean Titer
Result unit
007 Titration (EQP) [1] Formula R2=Mean[R1]
Titrant Constant C=1
Titrant EDTA M M[None]
Concentration 0.1 mol/L Z z[None]
Sensor Decimal places 5
Type Phototrode Result limits No
Sensor DP5 Record statistics Yes
Unit mV Send to buffer No
Temperature acquisition Condition No
Temperature measurement No
Stir
Speed 10%
Predispense
Mode None
Wait time 0 s
Control
Control User
Titrant addition Dynamic
dE (set value) 6.0 mV
dV (min) 0.01 mL
dV (max) 0.1 mL
Mode Equilibrium controlled
dE 1.0 mV
dt 3 s
t (min) 6 s
t (max) 30 s
Evaluation and recognition
Procedure Standard
Threshold 100
Tendency Negative
Ranges 0
Add. EQP criteria Steepest jump
Steepest jumps 1
Termination
At Vmax 7
At potential No
At slope No
After number of
recognized EQPs No
Combined termination
criteria No

METTLER TOLEDO Page 4 of 4 Titration Application M007

 METTLER TOLEDO Application M022
Titer Determination of EDTA 0.1 mol/L with Calcium Carbonate
Titer determination of EDTA by complexometric titration at pH 10 with calcium carbonate as a standard,
TM
Eriochrome Black T as color indicator and DP5 Phototrode (660 nm) as a photometric sensor.

Sample Calcium carbonate solution, Preparation and Procedures

c(CaCO3) = 0.1 mol/L
CAUTION
5.0 mL
‐ Use safety goggles, a lab coat and wear gloves.
Work in a fume hood.
Compound Calcium carbonate, CaCO3 ‐ Ensure accurate cleaning of sensor is sufficient
M = 100.09, z = 1 after each titration.
Sample titration:
Chemicals ‐ 40 mL deionized water ‐ Dispense 5 mL of 0.1 mol/L CaCO3 solution in a
‐ 10 mL Ammonia Buffer pH 10 titration beaker.
‐ Indicator: ‐ Add 0.1-0.2 mL of Eriochrome Black T solution
0.1 mL (≈3 drops) of 0.1% Erio T
(in ethanol)
‐ Start method
‐ Ethanol ‐ 10 mL Ammonia Buffer pH 10 is added from the
peristaltic pump.
Titrant Ethylenediaminetetraacetic acid ‐ 40 mL deionized water is added from the
disodium, EDTA-Na2 membrane pump.
C10H14N22Na2O8 x 2 H2O
‐ After stirring, titration is started
c(EDTA-Na2) = 0.1 mol/L ‐ Color change observed: red to violet.
‐ After completion of each sample, sensor, stirrer
Standard -- and titration tubes will be rinsed by deionized
water by means of membrane pump.
TM ‐ Subsequently, the sensor is cleaned in ethanol
Indication DP5 Phototrode (660 nm)
(color change: red-violet) in the conditioning beaker placed on the sample
changer rack.

Chemistry EDTA-Na2 + Ca
2+
 Remarks
EDTA-Ca + 2 Na
+
‐ Prior to use, adjust the output signal of the DP5
to approx. 1000 mV in deionized water by
Calculation R= m/(VEQ*c*C) turning the small knob on the housing.
C= 1/(cst*z) ‐ Rinsing and conditioning of the photometric
sensor is crucial to achieve accurate and precise
VEQ = Titrant consumption (mL) results.
c= Titrant concentration (mol/L)
cst = Concentration standard ‐ Rinse the photometric sensor with ethanol to
solution (mol/L) remove adherent material sticking on its mirror.
cst = 0.1 mol/L
m = Sample size (mL) ‐ Avoid formation of bubbles during titration by
z= Sample equivalent number keeping low speed rate of stirrer, as they disturb
the photometric indication.
‐ This method allows a fully automated analysis
procedure. The method can be modified for
Waste Neutralization of basic solution manual operation. Select “Manual stand” in the
disposal (pH 10 Ammonia) before final method function “Titration stand”.
disposal.

Author, Geeta Naik, IMSG

Version 2.0
Version Revised: C. De Caro, MSG AnaChem

METTLER TOLEDO Page 1 of 4 Titration Application M022

 Instruments ‐ Titration Excellence T50/T70/T90
(Other Titrators: with modification or manual operation are necessary)
‐ Rondo 20 Sample Changer with PowerShower™ (ME- 51108003)
‐ 1 x SP250 Peristaltic pump
‐ XP205 Balance

Accessories ‐ 100 mL PP Titration beakers (ME- 00101974)

®
‐ LabX pro titration software

Results
All results
Method-ID STDEDTACa
Sample CaCO3 (1/6)
R1 (1/6) 1.01165
Sample CaCO3 (2/6)
R1 (2/6) 1.01125
Sample CaCO3 (3/6)
R1 (3/6) 1.01151
Sample CaCO3 (4/6)
R1 (4/6) 1.01151
Sample CaCO3 (5/6)
R1 (5/6) 1.01055
Sample CaCO3 (6/6)
R1 (6/6) 1.01044

Statistics
Method-ID STDEDTACa
R1 6
Samples 6
Mean 1.0112
s 0.00053
srel 0.052%

Titration curve

METTLER TOLEDO Page 2 of 4 Titration Application M022

 Table of measured values
Volume Increment Signal Change 1st deriv. Time Temperature
mL mL mV mV mV/mL s °C
0.0000 NaN 655.7 NaN NaN 0 25.0
0.0100 0.0100 663.0 7.3 NaN 7 25.0
0.0200 0.0100 655.9 -7.1 NaN 14 25.0
0.0300 0.0100 664.0 8.1 NaN 20 25.0
0.0400 0.0100 662.3 -1.7 NaN 26 25.0
….. ….. ….. ….. ….. …… …..
4.7530 0.1000 729.5 -7.0 -137.62 326 25.0
4.8245 0.0715 722.1 -7.4 -287.11 339 25.0
4.8650 0.0405 710.9 -11.2 -540.36 346 25.0
4.8750 0.0100 706.4 -4.5 -814.05 353 25.0
4.8850 0.0100 698.2 -8.2 -1190.80 362 25.0
4.8950 0.0100 691.8 -6.4 -1578.17 370 25.0
4.9075 0.0125 676.7 -15.1 -1930.07 377 25.0
4.9175 0.0100 657.2 -19.5 -3513.06 383 25.0
4.9275 0.0100 627.4 -29.8 -6053.21 394 25.0
4.9375 0.0100 580.2 -47.2 -5068.81 400 25.0
EQP 4.942440 NaN 524.7 NaN -6421.96 NaN NaN
4.9475 0.0100 467.8 -112.4 -3783.44 413 25.0
4.9575 0.0100 364.7 -103.1 -3822.36 424 25.0
4.9675 0.0100 349.4 -15.3 -3182.25 434 25.0
4.9925 0.0250 346.0 -3.4 -1856.73 442 25.0
5.0550 0.0625 344.5 -1.5 -597.83 448 25.0
5.1550 0.1000 344,1 -0.4 -63.71 454 25.0
5.2550 0.1000 344.0 -0.1 0.98 460 25.0
5.3550 0.1000 344.3 0.3 2.75 466 25.0
5.4550 0.1000 344.4 0.1 2.21 472 25.0
….. ….. ….. ….. ….. ….. …..
6.4550 0.1000 344.8 -0.2 -1.01 533 25.0
6.5550 0.1000 344.8 0.0 -1.13 540 25.0
6.6550 0.1000 344.7 -0.1 NaN 546 25.0
6.7550 0.1000 344.3 -0.4 NaN 552 25.0
6.8550 0.1000 344.3 0.0 NaN 558 25.0
6.9550 0.1000 344.1 -0.2 NaN 564 25.0
7.0000 0.0450 343.7 -0.4 NaN 570 25.0

Comments

• Eriochrome Black T indicator solution:

Weigh 0.5 g of Eriochrome Black T in 100 mL volumetric flask, dissolve and make up the volume with
95% ethanol.

• Ammonia buffer pH 10:

Weigh 6.4 g of ammonium chloride in 100 mL volumetric flask, dissolve in 60 mL ammonia, and
make up the volume with deionized water.

METTLER TOLEDO Page 3 of 4 Titration Application M022

 Method

001 Title 008 Calculation R1

Type Titer determination Result Titer
Compatible with T50 / T70 / T90 Result unit --
ID STDEDTACa Formula R1=m/(VEQ*c*C)
Title Titer with EQP Constant C=1/(cst*z)
Author admin M M[None]
Date/Time . . . z z[None]
Modified on . . . Decimal places 5
Modified by admin Result limits No
Protect No Record statistics Yes
SOP None Extra statistical func. No
Send to buffer No
002 Sample (Titer) Condition No
Titrant EDTA
Concentration 0.1[mol/L] 009 Rinse
Standard CaCO3 Auxiliary reagent Water
Type of standard liquid Rinse cycles 1
Entry type Fixed volume Vol. per cycles 15 mL
Volume 5 mL Position Current position
Correction factor 1.0 Drain No
Temperature 25.0°C Condition No

003 Titration stand (Rondo/Tower A) 010 Conditioning

Type Rondo/Tower A Type Fix
Titration stand Rondo60/1A Interval 1
Lid handling No Position Conditioning beaker
Time 30 s
004 Pump Speed 10 %
Auxiliary reagent Buffer pH10 Condition No
Volume 10 mL
Condition No 011 End of sample

005 Pump 012 Titer

Auxiliary reagent Water Titrant EDTA
Volume 40 mL Concentration 0.1 mol/L
Condition No TITER Mean [R1]
Limits No
006 Stir Condition No
Speed 10 %
Duration 30 s 013 Calculation R2
Condition No Result Mean Titer
Result unit
007 Titration (EQP) [1] Formula R2=Mean[R1]
Titrant Constant C=1
Titrant EDTA M M[None]
Concentration 0.1 mol/L Z z[None]
Sensor Decimal places 5
Type Phototrode Result limits No
Sensor DP5 Record statistics Yes
Unit mV Send to buffer No
Temperature acquisition Condition No
Temperature measurement No
Stir
Speed 10%
Predispense
Mode None
Wait time 0 s
Control
Control User
Titrant addition Dynamic
dE (set value) 6.0 mV
dV (min) 0.01 mL
dV (max) 0.1 mL
Mode Equilibrium controlled
dE 1.0 mV
dt 3 s
t (min) 6 s
t (max) 30 s
Evaluation and recognition
Procedure Standard
Threshold 100
Tendency Negative
Ranges 0
Add. EQP criteria Steepest jump
Steepest jumps 1
Termination
At Vmax 7
At potential No
At slope No
After number of
recognized EQPs No
Combined termination
criteria No

METTLER TOLEDO Page 4 of 4 Titration Application M022

 METTLER TOLEDO Application M014
Titer of 0.1 mol/L EGTA
Method for the titer determination of EGTA using calcium carbonate solution as a standard. The
complexometric titration is monitored using a photometric sensor and a color indicator.

Sample Calcium carbonate solution, Preparation and Procedures

c(CaCO3) = 0.1 mol/L
5.0 mL CAUTION
• Use safety goggles, a lab coat, wear mask and
gloves. Work in a fume hood.
Compound Calcium carbonate, CaCO3
• Ensure accurate cleaning of sensor is sufficient
M = 100.09, z = 1
after each titration.
Chemicals ‐ 40 mL deionized water
‐ 10 mL ammonia buffer pH 10 Preparation:
‐ Indicator: • 0.1 mol/L EGTA solution:
0.1 mL (≈3 drops) of 0.1% Erio T
‐ Dissolve 9.51 g of EGTA in 50 mL deion.
(in ethanol)
water by adding 10 mol/L sodium hydroxide
until the solution is completely clear.
‐ Dilute up to 250 mL with deionized water.
Titrant Ethylene glycol tetraacetic acid, • 0.1 mol/L Calcium carbonate solution:
EGTA ‐ Weigh about 1.0009 g of CaCO3, dissolve it in
a few dilute hydrochloric acid.
c(EGTA) = 0.1 mol/L
‐ Dilute it to 100 mL with deionized water.
• 0.1% EBT indicator:
Standard --
‐ Weigh about 0.1 g of EBT indicator
‐ Dissolve and dilute it to 100 mL with ethanol.
TM • Buffer pH 10:
Indication DP5 Phototrode (660 nm)
‐ Weigh about 32.0 g of ammonium chloride,
add 300 mL of ammonia solution
2-
‐ Dilute up to 500 mL with deionized water.
Chemistry CaCO3 + [EGTA-H2] 
2-
[EGTA-Ca] + H2CO3 Procedure:
• Pipette 5.0 mL of calcium carbonate solution
Calculation R= m/(VEQ*c*C), and place the beaker on the sample changer.
C= 1/(cst*z)
• Add 1.0 mL EBT indicator.
VEQ= Titrant consumption (mL) • Start the method.
c = Titrant concentration (mol/L)
m= Sample size (mL) • 10 mL pH 10 buffer solution is added from the
cst = Concentration of standard the peristaltic pump
solution • 40 mL deionized water is dispensed from the
cst = 0.1 mol/L.
membrane pump.
z= Sample equivalent number
• After completion of each sample, sensor, stirrer
and titration tubes will be rinsed by deionized
Waste Neutralize the basic solution water by means of membrane pump.
disposal before disposal • Subsequently, the sensor is cleaned in ethanol
in the conditioning beaker placed on the
Author, Sohel Ansari, IMSG AnaChem, sample changer rack.
Version 1.0
Version Revised: C. De Caro, MSG AnaChem

METTLER TOLEDO Page 1 of 4 Titration Application M014

 Instruments ‐ Titration Excellence T50/T70/T90
(Other Titrators: depending on instrument type, manual operation and method
changes are necessary)
‐ Rondo 20 Sample Changer with PowerShower™ (ME- 51108003)
‐ XS205 Balance

Accessories ‐ 1 x SP250 Peristaltic pump (ME-51108016)

‐ 100 mL PP Titration beakers (ME-00101974)
®
‐ LabX pro titration software
‐ Spatula

Results

All results
Method-ID EGTA
Sample 5.0 mL (1/6)
R1 (CaCO3) 0.99446
Sample 5.0 mL (2/6)
R1 (CaCO3) 0.99371
Sample 5.0 mL (3/6)
R1 (CaCO3) 0.99472
Sample 5.0 mL (4/6)
R1 (CaCO3) 0.99023
Sample 5.0 mL (5/6)
R1 (CaCO3) 0.99599
Sample 5.0 mL (6/6)
R1 (CaCO3) 0.99578

Statistics
Method-ID EGTA
R1 Calcium carbonate (CaCO3)
Samples 6
Mean 0.99415
s 0.00210
srel 0.211 %

Titration curve

METTLER TOLEDO Page 2 of 4 Titration Application M014

 Table of measured values
Volume Increment Signal Change 1st deriv. Time Temperature
mL mL mV mV mV/mL s °C
0.0000 NaN 375.4 NaN NaN 0 25.0
0.1000 0.1000 412.2 36.8 NaN 3 25.0
0.2000 0.1000 416.1 3.9 NaN 6 25.0
0.3000 0.1000 416.9 0.8 NaN 9 25.0
0.4000 0.1000 418.5 1.6 NaN 12 25.0
0.5000 0.1000 418.9 0.4 -12.07 16 25.0
0.6000 0.1000 420.4 1.5 7.43 19 25.0
0.7000 0.1000 420.6 0.2 4.85 22 25.0
0.8000 0.1000 420.9 0.3 3.07 26 25.0
0.9000 0.1000 421.9 1.0 1.72 29 25.0
1.0000 0.1000 422.2 0.3 1.37 32 25.0
1.1000 0.1000 420.0 -2.2 3.34 35 25.0
1.2000 0.1000 422.9 2.9 3.99 38 25.0
1.3000 0.1000 422.2 -0.7 4.86 41 25.0
1.4000 0.1000 423.5 1.3 5.87 44 25.0
1.5000 0.1000 423.9 0.4 5.57 47 25.0
1.6000 0.1000 423.7 -0.2 2.42 50 25.0
------------------ --------------------- ------------- ---------------- -------------------- ---------- -------------------------
4.6000 0.1000 431.2 -0.3 -6.22 142 25.0
4.7000 0.1000 430.8 -0.4 -62.24 145 25.0
4.8000 0.1000 428.2 -2.6 -139.12 148 25.0
4.9000 0.1000 410.9 -17.3 -213.57 151 25.0
5.0000 0.1000 377.7 -33.2 -263.34 154 25.0
EQP1 5.063035 NaN 358.2 NaN -271.12 NaN NaN
5.1000 0.1000 346.7 -31.0 -273.79 157 25.0
5.2000 0.1000 322.3 -24.4 -242.52 161 25.0
5.3000 0.1000 303.5 -18.8 -185.69 164 25.0
5.4000 0.1000 288.6 -14.9 -134.03 167 25.0
5.5000 0.1000 277.0 -11.6 -102.27 171 25.0
5.6000 0.1000 268.0 -9.0 NaN 174 25.0
5.7000 0.1000 260.5 -7.5 NaN 177 25.0
5.8000 0.1000 254.8 -5.7 NaN 180 25.0
5.9000 0.1000 250.4 -4.4 NaN 183 25.0
6.0000 0.1000 246.7 -3.7 NaN 186 25.0

Comments

General:
‐ The mean value of the titer is automatically stored as part of the setup by the function TITER.
‐ This method allows a fully automated analysis procedure. The method can be modified for manual
operation. Select “Manual stand” in the method function “Titration stand”.

Procedure:
‐ Prior to use, adjust the output signal of the DP5 to approx. 1000 mV in deionized water by turning the
small knob on the housing.
‐ Avoid formation of bubbles during titration by keeping low speed rate of stirrer, as they disturb the
photometric indication.
‐ Rinsing and conditioning of the photometric sensor is crucial to achieve accurate and precise results.
Rinse the photometric sensor with ethanol to remove adherent material sticking on its mirror.

Literature:
Mettler-Toledo Application M014 (V1.0).

METTLER TOLEDO Page 3 of 4 Titration Application M014

 Method

001 Title 008 Calculation R1

Type Titer determination Result Titer
Compatible with T50 / T70 / T90 Result unit --
ID TiterofEGTA Formula R1=m/(VEQ*c*C)
Title Titer of 0.1 mol/L EGTA Constant C=1/(cst*z)
Author Administrator M M[Calcium carbonate]
....... z z[Calcium carbonate]
Decimal places 5
002 Sample (Titer) Result limits No
Titrant EGTA Record statistics Yes
Concentration 0.1 mol/L Extra statistical func. No
Standard CaCO3 Send to buffer No
Type of standard liquid Condition No
Entry type Fixed volume
Volume 5.0 mL 009 Rinse
Correction factor 1.0 Auxiliary reagent Water
Temperature 25.0°C Rinse cycles 1
Vol. per cycle 10 mL
003 Titration stand (Rondo/Tower A) Position Current position
Type Rondo/Tower A Drain No
Titration stand Rondo60/1A Condition No
Lid handling No
010 Conditioning
004 Pump Type Fix
Auxiliary reagent Buffer pH 10 Interval 1
Volume 10.0 mL Position Conditioning beaker
Condition No Time 10 s
Speed 30 %
005 Pump Condition No
Auxiliary reagent Water
Volume 40.0 mL 011 End of sample
Condition No
012 Titer
006 Stir Titrant EGTA
Speed 30 % Concentration 0.1
Duration 10 s TITER= Mean[R1]
Condition No Limits No
Condition No
007 Titration (EQP) [1]
Titrant 013 Calculation R2
Titrant EGTA Result Mean Titer
Concentration 0.1 mol/L Result unit --
Sensor Formula R2=Mean[R1]
Type Phototrode Constant C=1
Sensor DP5 M M[None]
Unit mV z z[None]
Temperature acquisition Decimal places 5
Temperature acquisition No Result limits No
Stir Record statistics Yes
Speed 20 % Extra statistical func. No
Predispense Send to buffer No
Mode None Condition No
Wait time 0 s
Control
Control User
Titrant addition Incremental
dV 0.1 mL
Mode Equilibrium controlled
dE 2.0 mV
dt 1 s
t (min) 3 s
t (max) 20 s
Evaluation and recognition
Procedure Standard
Threshold 100.0
Tendency Negative
Ranges 0
Add. EQP criteria No
Termination
At Vmax 10.0
At potential No
At slope No
After number of
recognized EQPs Yes
Number of EQPs 1
Combined termination
criteria No
Accompanying stating
Accompanying stating No
Condition
Condition No

METTLER TOLEDO Page 4 of 4 Titration Application M014

 METTLER TOLEDO Application M029
Titer Determination of Zinc Sulfate
Titer determination of zinc sulfate by complexometric titration at pH 10 with EDTA, Eriochrome Black T as
TM
color indicator, and DP5 phototrode (660 nm) as a photometric sensor.

Sample Volumetric solution Preparation and Procedures

5.0 mL EDTA Disodium solution
CAUTION
c(EDTA-Na2) = 0.1 mol/L
‐ Use safety goggles, a lab coat and wear gloves.
Work in a fume hood.
Compound EDTA-Na2 ‐ Ensure accurate cleaning of sensor is sufficient
M = 372.24, z = 1 after each titration.
Sample titration:
Chemicals ‐ 40 mL deionized water ‐ Dispense 5 mL of 0.1 mol/L EDTA solution in a
‐ 10 mL Ammonia Buffer pH 10 titration beaker.
‐ Indicator: ‐ Add 0.1-0.2 mL of Eriochrome Black T solution
0.1 mL (≈3 drops) of 0.1% Erio T
(in ethanol)
‐ Start method
‐ Ethanol ‐ 10 mL Ammonia Buffer pH 10 is added from the
peristaltic pump.
Titrant Zinc sulphate, ZnSO4 ‐ 40 mL deionized water is added from the
c(ZnSO4) = 0.1 mol/L membrane pump.
‐ After stirring, titration is started
‐ Color change observed: violet-red.
‐ After completion of each sample, sensor, stirrer
Standard -- and titration tubes will be rinsed by deionized
water by means of membrane pump.
TM ‐ Subsequently, the sensor is cleaned in ethanol
Indication DP5 Phototrode (660nm)
in the conditioning beaker placed on the sample
(color change: violet-red)
changer rack.

Chemistry EDTA-Na2 + Zn
2+
 Remarks
EDTA-Zn + 2 Na
+
‐ Prior to use, adjust the output signal of the DP5
to approx. 1000 mV in deionized water by
turning the small knob on the housing.
Calculation R= m/(VEQ*c*C)
C= 1/(cst*z) ‐ Rinsing and conditioning of the photometric
sensor is crucial to achieve accurate and precise
VEQ = Titrant consumption (mL) results.
c= Titrant concentration (mol/L)
m = Sample size (mL)
‐ Rinse the photometric sensor with ethanol to
cst = Concentration of standard remove adherent material sticking on its mirror.
solution (mol/L) ‐ Avoid formation of bubbles during titration by
cst = 0.1 mol/L
keeping low speed rate of stirrer, as they disturb
z= Sample equivalent number
the photometric indication.

Waste Zinc is precipitated with NaOH ‐ This method allows a fully automated analysis
or Ca(OH)2 and then filtered. procedure. The method can be modified for
disposal
Precipitate is classified as manual operation. Select “Manual stand” in the
special waste; the solution is method function “Titration stand”.
neutralized before final disposal
t
Author, Geeta Naik, IMSG
Version 2.0
Version Revised: C. De Caro, MSG AnaChem

METTLER TOLEDO Page 1 of 4 Titration Application M029

 Instruments ‐ Titration Excellence T50/T70/T90
(Other Titrators: with modification or manual operation are necessary)
‐ 1 x SP250 Peristaltic pump
‐ XP205 Balance

Accessories ‐ Rondo 20 Sample Changer with PowerShower™ (ME- 51108003)

‐ 100 mL PP Titration beakers (ME- 00101974)
®
‐ LabX pro titration software

Results
All results
Method-ID STDZnSO4
Sample EDTA (1/6)
R1 (1/6) 1.00874
Sample EDTA (2/6)
R1 (2/6) 1.00806
Sample EDTA (3/6)
R1 (3/6) 1.00929
Sample EDTA (4/6)
R1 (4/6) 1.01039
Sample EDTA (5/6)
R1 (5/6) 1.00968
Sample EDTA (6/6)
R1 (6/6) 1.00939

Statistics
Method-ID STDZnSO4
R1 6
Samples 6
Mean 1.009
s 0.00080
srel 0.079%

Titration curve

METTLER TOLEDO Page 2 of 4 Titration Application M029

 Table of measured values
Volume Increment Signal Change 1st deriv. Time Temperature
mL mL mV mV mV/mL s °C
0.0000 NaN 50.8 NaN NaN 0 25.0
0.0100 0.0100 50.8 0.0 NaN 6 25.0
0.0200 0.0100 50.9 0.1 NaN 12 25.0
0.0450 0.0250 50.9 0.0 NaN 18 25.0
0.1075 0.0625 50.9 0.0 NaN 24 25.0
0.2075 0.1000 51.4 0.5 3.98 30 25.0
0.3075 0.1000 52.0 0.6 3.81 36 25.0
0.4075 0.1000 52.3 0.3 3.45 43 25.0
0.5075 0.1000 52.6 0.3 3.04 49 25.0
0.6075 0.1000 52.8 0.2 2.68 55 25.0
…. ….. ….. ….. ….. ….. …..
4.3075 0.1000 63.4 0.4 3.67 280 25.0
4.4075 0.1000 63.8 0.4 1.66 286 25.0
4.5075 0.1000 64.3 0.5 -248.31 292 25.0
4.6075 0.1000 64.9 0.6 -166.34 298 25.0
4.7075 0.1000 65.9 1.0 158.77 301 25.0
4.8075 0.1000 67.3 1.4 899.18 311 25.0
4.9075 0.1000 73.8 6.5 2338.09 320 25.0
EQP 4.956668 NaN 334.7 NaN 3261.61 NaN NaN
4.9910 0.0835 516.9 443.1 4088.15 330 25.0
5.0010 0.0100 547.9 31.0 3632.35 337 25.0
5.0110 0.0100 568.8 20.9 2766.01 344 25.0
5.0210 0.0100 584.1 15.3 2499.12 350 25.0
5.0310 0.0100 595.8 11.7 1137.01 356 25.0
5.0410 0.0100 604.3 8.5 817.14 362 25.0
5.0510 0.0100 611.1 6.8 686.29 368 25.0
5.0620 0.0110 617.7 6.6 597.18 374 25.0
5.0735 0.0115 624.7 7.0 499.23 381 25.0
..... ….. ….. ….. ….. ….. …..
6.6605 0.1000 684.7 0.8 NaN 502 25.0
6.7605 0.1000 685.6 0.9 NaN 508 25.0
6.8605 0.1000 686.4 0.8 NaN 514 25.0
6.9605 0.1000 687.2 0.8 NaN 521 25.0
7.0000 0.0395 687.6 0.4 NaN 527 25.0

Comments

• Eriochrome Black T indicator solution:

Weigh 0.5 g of Eriochrome Black T in 100 mL volumetric flask, dissolve and make up the volume with
95% ethanol.

• Ammonia buffer pH 10:

Weigh 6.4 g of ammonium chloride in 100 mL volumetric flask, dissolve in 60 mL ammonia, and
make up the volume with deionized water.

METTLER TOLEDO Page 3 of 4 Titration Application M029

 Method

001 Title 008 Calculation R1

Type Titer determination Result Titer
Compatible with T50 / T70 / T90 Result unit
ID STDZNSO$ Formula R1=m/(VEQ*c*C)
Title Titer with EQP Constant C=1/(cst*z)
Author admin M M[None]
Date/Time . . . z z[None]
Modified on . . . Decimal places 5
Modified by admin Result limits No
Protect No Record statistics Yes
SOP None Extra statistical func. No
Send to buffer No
002 Sample (titer) Condition No
Titrant ZnSO4
Concentration 0.1[mol/L] 009 Rinse
Standard EDTA Auxillary reagent Water
Type of standard liquid Rinse cycles 1
Entry type Fixed volume Vol. per cycles 15 mL
Volume 5 mL Position Current position
Correction factor 1.0 Drain No
Temperature 25.0°C Condition No

003 Titration stand (Rondo/Tower A) 010 Conditioning

Type Rondo/Tower A Type Fix
Titration stand Rondo60/1A Interval 1
Lid handling No Position Conditioning beaker
Time 30 s
004 Pump Speed 10 %
Auxillary reagent Buffer pH10 Condition No
Volume 10 mL
Condition No 011 End of sample

005 Pump 012 Titer

Auxillary reagent Water Titrant ZnSO4
Volume 40 ml Concentration 0.1 mol/L
Condition No TITER Mean [R1]
Limits No
006 Stir Condition No
Speed 10 %
Duration 30 s 013 Calculation R2
Condition No Result Mean Titer
Result unit
007 Titration (EQP) [1] Formula R2=Mean[R1]
Titrant Constant C=1
Titrant ZnSO4 M M[None]
Concentration 0.1 mol/L Z z[None]
Sensor Decimal places 5
Type Phototrode Result limits No
Sensor DP5 Record statistics Yes
Unit mV Send to buffer No
Temperature acquisition Condition No
Temperature acquisition No
Stir
Speed 10%
Predispense
Mode None
Wait time 0 s
Control
Control User
Titrant addition Dynamic
dE (set value) 6.0 mV
dV (min) 0.01 mL
dV (max) 0.1 mL
Mode Equilibrium controlled
dE 1.0 mV
dt 3 s
t (min) 6 s
t (max) 30 s
Evaluation and recognition
Procedure Standard
Threshold 100
Tendency Positive
Ranges 0
Add. EQP criteria Steepestjump
Steepest jumps 1
Termination
At Vmax 7
At potential No
At slope No
After number of
recognized EQPs No
Combined termination
criteria No

METTLER TOLEDO Page 4 of 4 Titration Application M029

 METTLER TOLEDO Application M023
Titer Determination of Barium Perchlorate 0.005 mol/L
Titer determination of barium perchlorate by complexometric titration at pH 10 with EDTA, Phthalein
TM
purple as color indicator and DP5 Phototrode as a photometric sensor.

Sample 3.0 mL EDTA Disodium solution Preparation and Procedures

c(EDTA-Na2) = 0.01 mol/L
CAUTION
‐ Use safety goggles, a lab coat and wear gloves.
Work in a fume hood.
Compound EDTA-Na2, ‐ Ensure accurate cleaning of sensor is sufficient
C10H14N22Na2O8 x 2H2O after each titration.
M = 372.24, z = 1
Sample titration:
Chemicals ‐ Methanol:water 1:1 v/v ‐ Dispense 3 mL 0.01 mol/L EDTA solution in a
‐ 5 mL 2% ammonia solution titration beaker.
‐ Indicator:
0.2 mL 0.1% Phthalein purple (in
‐ Add 0.2 mL 0.1% phthalein purple solution
1 M sodium acetate) ‐ Start method
‐ Methanol ‐ 50 mL methanol:water (1:1) is added with the
membrane pump of sample changer.
Titrant Barium perchlorate, Ba(ClO4)2 ‐ 5 mL ammonia buffer pH 10 is added from the
in isopropanol:water (8:2) peristaltic pump.
‐ After stirring, titration is started
c(Ba(ClO4)2) = 0.005 mol/L ‐ Color change observed: colorless-purple.
‐ After completion of each sample, sensor, stirrer
Standard -- and titration tubes will be rinsed with
methanol:water by means of membrane pump.
‐ Subsequently, the sensor is cleaned in methanol
TM in the conditioning beaker placed on the sample
Indication DP5 Phototrode (555 nm)
photometric sensor changer rack.

Remarks
Chemistry Ba(ClO4)2 + EDTA-Na2 
EDTA-Ba + 2 NaClO4 ‐ Prior to use, adjust the output signal of the DP5
to approx. 1000 mV in deionized water by
turning the small knob on the housing.
Calculation R = m/(VEQ*c*C)
C= 1/(cst*z) ‐ Rinsing and conditioning of the phototrode is
crucial to achieve accurate and precise results.
VEQ = Titrant consumption (mL)
‐ Avoid formation of bubbles during titration by
c= Titrant concentration (mol/L)
m = Sample size (mL) keeping low speed rate of stirrer, as they disturb
cst = Concentration of standard the photometric indication.
solution
‐ To avoid formation of bubbles during titration the
cst = 0.01 mol/L
mixture of methanol, water and indicator is
z= Sample equivalent number
degassed in an ultrasonic bath for 5 mins.
Waste Neutralization before final ‐ This method allows a fully automated analysis
disposal disposal as special waste procedure. The method can be easily modified
for manual operation. Select “Manual stand” in
the method function “Titration stand”.
Author, Robin Isyas, IMSG
Version 2.0
Version Revised: C. De Caro, MSG AnaChem

METTLER TOLEDO Page 1 of 4 Titration Application M023

 Instruments ‐ Titration Excellence T50/T70/T90
(Other Titrators: with modification or manual operation are necessary)
‐ XP205 Balance
‐ 1 x 10 mL DV1010 glass burette (ME-51107501)

TM
Accessories ‐ Rondo 20 with Power shower (ME-51108003)
‐ 100 mL PP Titration beakers (ME-00101974)
‐ 1 x Peristaltic pump SP250
®
‐ LabX pro titration software

Results

All results
Method-ID Titre
Sample EDTA (1/6)
R1 (1/6) 1.00727
Sample EDTA (2/6)
R1 (2/6) 1.01142
Sample EDTA (3/6)
R1 (3/6) 1.00577
Sample EDTA (4/6)
R1 (4/6) 1.01151
Sample EDTA (5/6)
R1 (5/6) 1.00973
Sample EDTA (6/6)
R1 (6/6) 1.01241

Statistics
Method-ID Titre
R1 6
Samples 6
Mean 1.0097
s 0.00264
srel 0.262 %

Titration curve

METTLER TOLEDO Page 2 of 4 Titration Application M023

 Table of measured values
Volume Increment Signal Change 1st deriv. Time Temperature
mL mL mV mV mV/mL s °C
0.0000 NaN 989.8 NaN NaN 0 25.0
5.0000 5.0000 1.001.7 11.9 NaN 16 25.0
5.0500 0.0500 1001.8 0.1 NaN 82 25.0
5.1000 0.0500 1001.8 0.0 NaN 88 25.0
5.1500 0.0500 1002.0 0.2 NaN 93 25.0
5.2000 0.0500 1001.6 -0.4 1.37 99 25.0
5.2500 0.0500 1002.1 0.5 1.69 104 25.0
5.3000 0.0500 1002.2 0.1 2.92 109 25.0
5.3500 0.0500 1001.9 -0.3 2.67 114 25.0
5.4000 0.0500 1002.5 0.6 0.83 119 25.0
5.4500 0.0500 1002.4 -0.1 -1.36 124 25.0
5.5000 0.0500 1002.5 0.1 -0.73 130 25.0
… …. …. …. …. … …..
5.7500 0.0500 1002.7 0.0 4.87 159 25.0
5,8000 0.0500 1003.0 0.3 4.11 165 25.0
5.8500 0.0500 1003.0 0.0 15.74 170 25.0
5.9000 0.0500 1003.2 0.2 24.48 176 25.0
5.9500 0.0500 1003.6 0.4 6.74 181 25.0
6.0000 0.0500 1003.5 -0.1 -54.24 187 25.0
6.0500 0.0500 1003.3 -0.2 -152.43 194 25.0
6.1000 0.0500 992.4 -10.9 -268.59 199 25.0
6.1500 0.0500 973.8 -18.6 -374.58 205 25.0
6.2000 0.0500 950.6 -23.2 -443.00 211 25.0
6.2500 0.0500 927.7 -22.9 -461.28 218 25.0
EQP 6.254515 NaN 925.7 NaN -465.83 NaN NaN
6.3000 0.0500 905.8 -21.9 -432.21 223 25.0
6.3500 0.0500 885.6 -20.2 -389.52 229 25.0
6.4000 0.0500 867.7 -17.9 -346.51 236 25.0
6.4500 0.0500 851.2 -16.5 -308.46 241 25.0
6.5000 0.0500 837.0 -14.2 NaN 246 25.0
6.5500 0.0500 823.9 -13.1 NaN 252 25.0
6.0000 0.0500 812.4 -11.5 NaN 257 25.0
6.6500 0.0500 802.3 -10.1 NaN 262 25.0
6.7000 0.0500 793.0 -9.3 NaN 267 25.0

Comments

• Phthalein purple indicator solution :

Weigh 0.1 g of phthalein purple in 100mL volumetric flask, dissolve and make up the volume with
1 M sodium acetate.

• 1 M Sodium acetate :
Weigh 8.203 g of sodium acetate in 100 mL volumetric flask, and make up the volume with deionized
water.

METTLER TOLEDO Page 3 of 4 Titration Application M023

 Method

001 Title 008 Calculation R1

Type Titer determination Result Titer
Compatible with T50/T70/T90 Result unit --
ID Titre Formula R1=m/(VEQ*c*C)
Title Barium perchlorate Constant C=1/(cst*z)
Author admin M M[None]
. . . . . . z z[None]
SOP None Decimal places 5
Result limits No
002 Sample (Titer) Record statistics yes
Titrant Barium perchlorate Extra statistical func. No
Concentration 0.005 mol/L Send to buffer No
Standard EDTA Condition No
Type of standard liquid
Entry type Fixed volume 009 Rinse
Volume 3.0 mL Auxiliary reagent Water:methanol
Correction factor 1.0 Rinse cycles 1
Temperature 25.0°C Vol. per cycles 15 mL
Position Current position
003 Titration stand (Rondo/Tower A) Drain No
Type Rondo/Tower A Condition No
Titration stand Rondo60/1A
Lid handling No 010 Conditioning
Type Fix
004 Pump Interval 1
Auxiliary reagent Water:methanol Position conditioning beaker
Volume 50 mL Time 40 s
Condition No Speed 20 %
Condition No
005 Pump
Auxiliary reagent Ammonia 011 End of sample
Volume 5 mL
Condition No 012 Titer
Titrant Barium perchlorate
006 Stir Concentration 0.005 mol/L
Speed 20 % TITER Mean [R1]
Duration 30 s Limits No
Condition No Condition No

007 Titration (EQP) [1] 013 Calculation R2

Titrant Result Mean Titer
Titrant Barium perchlorate Result unit --
Concentration 0.005 mol/L Formula R2=Mean[R1]
Sensor Constant C=1
Type Phototrode M M[None]
Sensor DP5 Z z[None]
Unit mV Decimal places 5
Temperature acquisition Result limits No
Temperature measurement No Record statistics Yes
Stir Send to buffer No
Speed 10% Condition No
Predispense
Mode Volume
Volume 5.0 mL
Wait time 60 s
Control
Control User
Titrant addition Incremental
dV 0.05 mL
Mode Equilibrium controlled
dE 0.5 mV
dt 3 s
t (min) 5 s
t (max) 30 s
Evaluation and recognition
Procedure Standard
Threshold 100 mV/mL
Tendency Negative
Ranges 0
Add. EQP criteria Steepest jump
Steepest jumps 1
Termination
At Vmax 8
At potential No
At slope No
After number of
recognized EQPs Yes
Number of EQPs 1
Combined termination
criteria No
Accompanying stating
Accompanying stating No
Condition
Condition No

METTLER TOLEDO Page 4 of 4 Titration Application M023