Title Applications Brochure 4 - METTLER TOLEDO · PDF fileApplications Brochure ... Determination of Copper M063. ... If cyanide is present in the sample the addition of a sulfuric

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METTLER TOLEDO Electroplating Industry

Contents

Method Title Electroless Copper Bath M062 Electroless copper bath: Determination of Copper

M063 Electroless copper bath: Free Complexing agents

M064 Electroless copper bath: Sodium Hydroxide and Formaldehyde Electroless Nickel Bath

M065 Electroless Nickel Bath: Determination of Sodium Hypophosphite

M066 Electroless Nickel Bath: Determination of Nickel

M067 Electroless Nickel Bath: Determination of Sodium Orthophosphite

METTLER TOLEDO Page 1 of 4 Titration Application M062

METTLER TOLEDO Application M062

Electroless Copper Bath: Determination of Copper Method for determination of copper in electroless copper bath by iodometric titration.

Preparation and Procedures CAUTION ‐ Use safety goggles, a lab coat, wear mask and

gloves. Always work in a fume hood. ‐ Ensure cleaning of sensor after each titration.

Sample Preparation: Electroless copper bath ‐ Take 158 mL deionized water in 200 mL

volumetric flask add 2 mL Cu-bath Ginplate Cu 406-C with stirring.

‐ While stirring add 20mL Ginplate Cu 406-B and 20 mL Ginplate Cu 406-A.

(Literature: GINPLATE CU 406)

Sample titration: ‐ Dispense 10 mL of sample from additional

dosing unit to the titration beaker placed on sample changer.

‐ Add 40 mL of 25% H2SO4 from peristaltic pump. ‐ Add 5 mL of 10% KI from additional dosing unit. ‐ Add 5 mL of 10% KSCN from additional dosing

unit. ‐ Wait for 5 minutes with stirring ‐ Titrate with 0.1mol/L Na2S2O3. ‐ After completion of each sample, sensor, stirrer

and titration tubes are rinsed by deionized water by means of membrane pump.

‐ Sensor is cleaned with deionized water in conditioning beaker placed on sample changer after each sample.

Remarks

‐ The method parameters have been optimized for the sample of this application. It may be necessary to adapt the method to your specific sample.

‐ This method allows a fully automated analysis procedure. This method can be easily modified for manual operation. Select “Manual stand” in the method function “Titration stand”

‐ Purity of potassium iodate used is 99.5%.

Literature: ‐ Ginplate Cu 406, (www.growel.com/tds/796.pdf ),

a trademark of Grauer & Weil India Ltd, www.growel.com ‐ Mettler-Toledo Applications M062 and M009.

Sample Electroless copper bath,10 mL (see “Preparation”)

Compound Copper (Cu2+), M = 63.54 g/mol, z = 1,

Copper Sulfate (CuSO4), M= 159.60 g/mol, z = 1,

Copper Sulfate Pentahydrate (CuSO4.5H2O), M = 249.68 g/mol, z = 1

Chemicals 25% Sulfuric acid, 40 mL 10% Potassium iodide, KI, 5 mL 10% Potassium thiocyanate, KSCN, 5 mL.

Titrant Sodium thiosulfate, Na2S2O3 c(Na2S2O3) = 0.1 mol/L

Standard Potassium iodate, KIO3 20-30 mg

Indication DMi140-SC (Combined platinum ring redox electrode)

Chemistry 2CuSO4 + 4KI + → 2CuI + 2K2SO4 + I2 2Na2S2O3 + I2 → Na2S4O6 + 2NaI

Calculation R1 = Q*C/m, g/L (Cu content) R2 = Q*C/m, g/L (CuSO4) R2 = Q*C/m, g/L (CuSO4•5H2O) C = M/z Q = Titrant consumption in mmol. m = mass of the sample in mL M = Molar mass of sample in g. z = Equivalent number of sample

Waste disposal

Copper solutions : If necessary, neutralize the solution before final disposal as special waste

Author, Version

Ruby Das, IMSG AnaChem, Version 2.0, Revised: C. De Caro, MSG AnaChem

http://(www.growel.com/tds/796.pdf

http://www.growel.com/


Instruments ‐ Titration Excellence T70/T90 (Other Titrators: depending on instrument type, manual operation and method changes are necessary)

‐ Rondo 20 Sample Changer with PowerShowerTM (MT-51108003) ‐ XP 205 Balance

Accessories ‐ 3 x Additional dosing unit (MT-51109030) ‐ 3 x 10 mL DV1010 glass burette (MT-51107501) ‐ 1 x 5 mL DV1005 glass burette (MT-51107500) ‐ 100 mL Polypropylene titration beakers (MT-00101974) ‐ Peristaltic pump SP250 (MT-51108016) ‐ LabX® pro titration software

Results Results Method-ID Copper Sample 10 mL (1/6) Cu 2.663 g/L CuSO4 6.688 g/L CuSO4.5H2O 10.463 g/L Sample 10 mL (2/6) Cu 2.663 g/L CuSO4 6.689 g/L CuSO4.5H2O 10.464 g/L Sample 10 mL (3/6) Cu 2.668 g/L CuSO4 6.701 g/L CuSO4.5H2 10.483 g/L Sample 10 mL (4/6) Cu 2.668 g/L CuSO4 6.702 g/L CuSO4.5H2O 10.485 g/L Sample 10 mL (5/6) Cu 2.663 g/L CuSO4 6.688 g/L CuSO4.5H2O 10.463 g/L Sample 10 mL (6/6) Cu 2.664 g/L CuSO4 6.692 g/L CuSO4.5H2O 10.469 g/L Statistics Method-ID Copper R1 Copper Samples 6 Mean 2.665 g/L s 0.002 g/L srel 0.093 % R2 CuSO4 Samples 6 Mean 6.693 g/L s 0.007 g/L srel 0.097 % R3 CuSO4.5H2O Samples 6 Mean 10.471 g/L s 0.010 g/L srel 0.097 %

Titration curve


Table of measured values

Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C

0.0000

NaN

351.1

NaN

NaN

0

25.0

1.0000 0.1000 348.3 -2.8 NaN 4 25.0 1.1000 0.1000 347.3 -1.0 NaN 7 25.0 1.2000 0.1000 347.0 -0.3 NaN 10 25.0 1.3000 0.1000 346.6 -0.4 NaN 13 25.0 1.4000 0.1000 346.3 -0.3 -4.94 16 25.0 1.5000 0.1000 345.8 -0.5 -4.69 19 25.0 1.6000 0.1000 345.3 -0.5 -6.07 22 25.0 1.7000 0.1000 344.6 -0.7 -6.78 25 25.0 1.8000 0.1000 343.9 -0.7 -7.19 28 25.0 1.9000 0.1000 343.1 -0.8 -7.18 31 25.0 2.0000 0.1000 342.4 -0.7 -7.00 34 25.0 2.1000 0.1000 341.8 -0.6 -6.79 37 25.0 2.2000 0.1000 341.1 -0.7 -6.78 40 25.0 2.3000 0.1000 340.4 -0.7 -7.02 43 25.0 --------- ----------------- ---------- ------------ --------------- -------- ------------------------ 3.8000 0.1000 320.0 -2.8 -33.46 89 25.0 3.9000 0.1000 316.5 -3.5 -76.65 92 25.0 4.0000 0.1000 311.1 -5.4 -122.03 96 25.0 4.1000 0.1000 301.5 -9.6 -153.00 104 25.0

EQP1 4.169456 NaN 279.8 NaN -159.19 NaN NaN 4.2000 0.1000 270.3 -31.2 -158.95 122 25.0 4.3000 0.1000 255.3 -15.2 -138.10 130 25.0 4.4000 0.1000 248.4 -6.9 -97.40 134 25.0 4.5000 0.1000 243.5 -4.9 -52.08 139 25.0 4.6000 0.1000 240.1 -3.4 -21.68 142 25.0 4.7000 0.1000 237.1 -3.0 NaN 145 25.0 4.8000 0.1000 234.4 -2.7 NaN 148 25.0 4.9000 0.1000 232.0 -2.4 NaN 151 25.0 5.0000 0.1000 230.0 -2.0 NaN 154 25.0 5.1000 0.1000 228.1 -1.9 NaN 157 25.0

Comments

• Be careful! If cyanide is present in the sample the addition of a sulfuric acid solution must be performed in a ventilated fume hood (formation of poisonous HCN!).

• This electroless copper bath is used for chemical copper deposition on printed circuit boards. It consists of sodium hydroxide, formaldehyde, weakly complexed copper, free complexing agent(s), and additives.

• Titer determination of 0.1 mol/L Na2S2O3 is done as per the Mettler-Toledo application M009 and mean value found is 1.00509. The mean value of the titer is automatically stored as part of the setup by the function TITER.

Principle : ‐ A weaker copper complex is decomposed at room temperature by the acid medium. A stronger

complex is decomposed in the same way at elevated temperature. ‐ After decomposition the sample is cooled at room temperature. ‐ Then potassium iodide (KI) and potassium thiocyanate (KSCN) are added. ‐ Cu(II) is reduced with excess iodide (I-) and subsequently precipitated as CuI in the presence of

thiocyanate (SCN-). KSCN is added to avoid adsorption of I2 on the surface of CuI :

2Cu2+ + 4I- → 2CuI + I2

‐ The amount of iodine formed is proportional to the Cu (II) content. Cover the beakers to avoid loss of iodine. The complete reduction of Cu (II) requires 5 min.

‐ The liberated I2 is then titrated at room temperature with Na2S2O3.

2 S2O32- + I2 → S4O6

2- + 2I-

‐ Stir moderately. Vigorous stirring causes loss of I2. ‐ Alternative: Photometric indication with DP5 PhototrodeTM ; indicator : starch


Method 001 Title Type General titration Compatible with T70/T90 ID Copper Title Determination of copper Author admin ...... 002 Sample Number of IDs 1 ID 1 Copper Entry type Fixed volume Volume 10.0 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C 003 Titration stand (Rondo/TowerA) Type Rondo/TowerA Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant CU SAMPLE Concentration 1 Volume 10.0 mL Dosing rate 60.0 mL/min Condition No 005 Pump Auxiliary reagent H2SO4 25% Volume 40.0 mL Condition No 006 Dispense (normal) [2] Titrant 10% KI Concentration 1 Volume 5.0 mL Dosing rate 60.0 mL/min Condition No 007 Dispense (normal) [3] Titrant 10% KSCN Concentration 0.1 Volume 5.0 mL Dosing rate 60.0 mL/min Condition No 008 Stir Speed 40 % Duration 10 s Condition No 009 Instruction Instruction 1 Mode Time interval Time interval 300 s Print Yes LabX command No Condition No 010 Titration (EQP) [1] Titrant Titrant Na2S2O3 Concentration 0.1 mol/L Sensor Type mV Sensor DM140-SC Unit mV Temperature acquisition Temperature acquisition No Stir Speed 40 % Predispense Mode Volume Volume 1.0 mL Wait time 0 Control Control User Titrant addition Incremental dV 0.1 mL Mode Equilibrium controlled dE 0.5 mV dt 1.0 s t (min) 3.0 s t (max) 30.0 s

Evaluation and recognition Procedure Standard Threshold 100.0 mV/mL Tendency Negative Ranges 0 Add. EQP criteria No Termination At Vmax 10.0mL 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 011 Calculation R1 Result Cu Result unit g/L Formula R1=Q*C/m Constant C=M/z M M[Copper] z z[Copper] Decimal places 3 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 012 Calculation R2 Result CuSO4 Result unit g/L Formula R2=Q*C/m Constant C=M/z M M[Copper sulphate] z z[Copper sulphate] Decimal places 3 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 013 Calculation R3 Result CuSO4.5H2O Result unit g/L Formula R3=Q*C/m Constant C=M/z M M[Copper sulphate

pentahydrate] z z[Copper sulphate

pentahydrate] Decimal places 3 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 014 Rinse Auxiliary reagent WATER Rinse cycles 1 Vol.per cycle 10.0 mL Position Current position Drain No Condition No 015 Conditioning Type Fix Interval 1 Position Conditioning beaker Time 10s Speed 30% Condition No 016 End of sample



Electroless Copper Bath: Determination of Free Complexing Agents Method for determination of free complexing agents in electroless copper bath.

Preparation and Procedures CAUTION ‐ Use safety goggles, a lab coat and wear gloves. If possible,

work in a fume hood. ‐ Ensure accurate cleaning of sensor is sufficient after each

titration. Sample Preparation : ‐ Electroless copper bath: Take 158 mL deionized water in

200 mL volumetric flask add 2 mL Ginplate Cu 406-Cwith stirring. While stirring add 20 mL Ginplate Cu 406-B and 20 mL Ginplate Cu 406-A. (Literature : Ginplate CU 406)

Sample titration : ‐ Add 0.2 g murexide trituration with NaCl (1:500) in the

beaker placed on sample changer. ‐ Dispense 5 mL of sample from additional dosing unit . ‐ Add 60 mL of deionized water from additional dosing unit. ‐ The sample is enough alkaline, and therefore no pH buffer is

needed for the pH adjustment in the alkaline region necessary for EDTA titration .

‐ Titrate with 0.01 mol/L CuSO4. ‐ After completion of each sample sensor, stirrer and titration

tubes are rinsed by deionized water by means of membrane pump.

‐ Sensor is cleaned with deionized water in the conditioning beaker placed on sample changer after each sample.

Remarks

‐ Prior to use , adjust the output signal of the DP5 PhototrodeTM to approx.. 1000 mV in deionized water before starting titration (100% transmission) by turning the small knob on the housing.

‐ Rinsing and conditioning of the Phototrode is crucial to achieve accurate and precise results.

‐ Avoid formation of bubbles during titration by low speed rate of stirrer, as they disturb photometric indication.

‐ This method allows a fully automated analysis procedure. This method can be easily modified for manual operation. Select “Manual stand” in the method function “Titration stand”.

‐ Sample may be dispensed manually using a pipette instead of using an additional dosing unit.

Literature : ‐ Ginplate Cu 406, ( http://www.growel.com/tds/796.pdf), a

trademark of Grauer & Weil India Ltd, www.growel.com ‐ Mettler – Toledo Application M063

Sample Electroless copper bath, 5 mL

Compound Free complexing agents

Chemicals Deionized water, 60 mL Indicator: 0.2 g Murexide trituration with NaCl (1:500).

Titrant Copper Sulfate, CuSO4

c(CuSO4) = 0.01 mol/L

Standard Ethylenediaminetetraacetic acid disodium,C10H14N2Na2O8 • 2H2O c(EDTA- Na2) = 0.01 mol/L

Indication DP5 PhototrodeTM (555 nm) (violet to yellow color)

Chemistry Cu2+ + Agent → Cu-Agent2+

At equivalence point : Cu2++ Murexide- → Cu-Murexide+

Calculation R = Q*C/m*d, mol/L Q = Titrant consumption in mmol C = 1000 d = Density of sample in g/mL m = Mass of sample in mL

Waste disposal

Copper solutions: If necessary, neutralize the solution before final disposal as special waste.

Author, Version

Ruby Das, IMSG AnaChem, V2.0 Revised: C. De Caro, MSG AnaChem

http://www.growel.com/tds/796.pdf



Instruments ‐ Titration Excellence T50/T70/T90 (Other Titrators: depending on instrument type, manual operation and method changes are necessary)

‐ XP205 Balance (MT-1106024) ‐ Rondo 20 with PowerShowerTM (MT-51108003)

Accessories ‐ 2 x Additional dosing unit (MT-51109030) ‐ 1 x 20 mL DV1020 glass burette (MT-51107502) ‐ 1 x 10 mL DV1010 glass burette (MT-51107501) ‐ 1 x 5 mL DV 1005 glass burette (MT-51107500) ‐ 100 mL Propylene titration beakers (MT-00101974) ‐ LabX® pro titration software

Results All results Method-ID FCA Sample 5 mL (1/6) R1 (Free complexing agents) 5.773 mmol/L Sample 5 mL (2/6) R2 (Free complexing agents) 5.762 mmol/L Sample 5 mL (3/6) R3 (Free complexing agents) 5.739 mmol/L Sample 5 mL (4/6) R4 (Free complexing agents) 5.758 mmol/L Sample 5 mL (5/6) R5 (Free complexing agents) 5.767 mmol/L Sample 5 mL (6/6) R6 (Free complexing agents) 5.758 mmol/L Statistics Method-ID FCA R1 Free complexing agents Samples 6 Mean 5.760 s 0.012 srel 0.201%

Titration curve


Table of measured values Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C 0.0000 NaN 142.1 NaN NaN 0 25.0 0.1000 0.1000 141.9 -0.2 NaN 3 25.0 0.2000 0.1000 141.8 -0.1 NaN 6 25.0 0.3000 0.1000 141.4 -0.4 NaN 9 25.0 0.4000 0.1000 141.3 -0.1 NaN 12 25.0 0.5000 0.1000 141.2 -0.1 -1.75 15 25.0 0.6000 0.1000 141.0 -0.2 -1.70 18 25.0 0.7000 0.1000 140.8 -0.2 -1.78 21 25.0 0.8000 0.1000 140.6 -0.2 -2.16 24 25.0 0.9000 0.1000 140.4 -0.2 -2.37 27 25.0 1.0000 0.1000 140.2 -0.2 -2.20 30 25.0 1.1000 0.1000 139.9 -0.3 -2.17 34 25.0 1.2000 0.1000 139.7 -0.2 -2.02 37 25.0 1.3000 0.1000 139.5 -0.2 -1.82 40 25.0 1.4000 0.1000 139.5 0.0 -1.20 43 25.0 ------------ ------------------- --------- ----------- --------------- ------ ----------- 2.5000 0.1000 146.8 4.4 64.12 78 25.0 2.6000 0.1000 152.0 5.2 132.23 83 25.0 2.7000 0.1000 166.6 14.6 207.50 87 25.0 2.8000 0.1000 191.1 24.5 260.65 92 25.0 EQP1 2.884740 NaN 219.7 NaN 274.61 NaN NaN 2.9000 0.1000 224.8 33.7 274.47 98 25.0 3.0000 0.1000 255.4 30.6 245.25 105 25.0 3.1000 0.1000 275.4 20.0 182.47 111 25.0 3.2000 0.1000 285.5 10.1 111.63 118 25.0 3.3000 0.1000 292.6 7.1 56.08 124 25.0 3.4000 0.1000 297.6 4.4 NaN 129 25.0 3.5000 0.1000 299.7 2.7 NaN 134 25.0 3.6000 0.1000 300.5 0.8 NaN 137 25.0 3.7000 0.1000 301.8 1.3 NaN 140 25.0 3.8000 0.1000 302.4 0.6 NaN 143 25.0

Comments

Standardization of 0.01M CuSO4 : ‐ Take 5 mL of 0.01M EDTA in a titration beaker. ‐ Add 50 mL deionized water. ‐ Add 0.1 g murexide trituration with NaCl (1: 500) with stirring. ‐ Titrate with 0.01M CuSO4. ‐ Sensor used: DP5 PhototrodeTM (555nm). The color change observed is from pink to yellow. ‐ Titer determination of 0.01 mol/L CuSO4 is done and mean value found is 0.97902. The mean value of

the titer is automatically stored as part of the setup by the function TITER. Sample titration: ‐ The copper bath is diluted and then titrated with 0.01M Cu(II) titrant. No pH buffer is added, the sample

is alkaline. ‐ It is recommended to use a murexide trituration with NaCl.(1:500). Add the indicator just before starting

analysis. ‐ Keep sample free of air bubbles during titration. Air bubbles and undissolved impurities affect the

photometric indication. ‐ Due to the steep signal change, an EQP titration with fixed increments is used. The low threshold

value allows for different amounts of indicator. ‐ Titration time: approx. 4 minutes. A fixed predispensing shortens the titration time Principle : ‐ Free complexing agents are titrated with Cu(II) solution in alkaline solution:

Cu2+ + Agent → Cu-Agent2+ ‐ At the equivalence point (simplified):

Cu2+ + Murexide- → Cu-Murexide+ (violet to yellow)


Method 001 Title Type General titration Compatible with T50 / T70 / T90 ID FCA Title Free complexing agents . . . 002 Sample Number of IDs 1 ID 1 Free complexing agents Entry type Fixed volume Volume 5.0 mL Density 1.0220 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary 003 Titration stand (Rondo/TowerA) Type Rondo/TowerA Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant CU SAMPLE Concentration 1 Volume 5.0 mL Dosing rate 60.0 mL/min Condition No 005 Dispense (normal) [2] Titrant WATER Concentration 100 Volume 60.0 mL Dosing rate 60.0 mL/min Condition No 006 Stir Speed 10% Duration 120 s Condition No 007 Titration (EQP) [1] Titrant Titrant CuSO4 Concentration 0.01 mol/L Sensor Type Phototrode Sensor DP5 Unit mV Temperature acquisition Temperature measurement No Stir Speed 10% Predispense Mode None Wait time 0 s Control Control User Titrant addition Incremental dV 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 2 s t (min) 3 s t (max) 30 s Evaluation and recognition Procedure Standard Threshold 100.0 mV/mL Tendency Positive Ranges 0 Add. EQP criteria No Termination At Vmax 30.0 mL At potential Yes Potential 1000 Termination tendency None 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

008 Calculation R1 Result Free complexing agents Result unit mmol/L Formula R1= Q1*C/m*d Constant C=1000 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 009 Rinse Auxillary reagent WATER Rinse cycles 1 Vol.per cycle 10 mL Position Current position Drain No Condition No 010 Condition Type Fix Interval 1 Position Conditioning beaker Time 20 s Speed 10 % Condition No 011 End of sample


METTLER TOLEDO Application M064 Electroless Copper Bath: Determination of Sodium Hydroxide and Formaldehyde Content

Method for determination of sodium hydroxide and formaldehyde content in electroless copper bath.

Preparation and Procedures CAUTION ‐ Use safety goggles, a lab coat and wear gloves. If possible,

work in a fume hood. ‐ Ensure accurate cleaning of sensor is sufficient after each

titration. Sample Preparation : ‐ Electroless copper bath: Take 158 mL deionized water in

200 mL volumetric flask add 2 mL Ginplate Cu 406-Cwith stirring. While stirring add 20 mL Ginplate Cu 406-B and 20 mL Ginplate Cu 406-A. (Literature : Ginplate CU 406)

Sample titration : ‐ Dispense 5mL of sample from additional dosing unit in the

titration beaker placed on sample changer. ‐ Add 50 mL of deionized water from additional dosing unit. ‐ Titrate with 0.1 mol/L HCl till the endpoint (i.e. pH = 10.5). ‐ pH of Na2SO3 solution is first adjusted to 10.5 to avoid

complicated blank correction. ‐ Dispense 10 mL of 1.0 mol/L Na2SO3 (pH = 10.5) from

additional dosing unit with stirring. ‐ Titrate with 0.1mol/L HCl. ‐ After completion of each sample sensor, stirrer and titration

tubes are rinsed by deionized water by means of membrane pump.

‐ Sensor is cleaned with deionized water in the conditioning beaker placed on sample changer after each sample.

‐ The nominal concentration of sodium hydroxide (NaOH) is given in the auxillary value H[Nominal value of NaOH].

‐ The nominal concentration of formaldehyde (HCHO) is given in the auxillary value H[Nominal value of HCHO].

Remarks ‐ The method parameters have been optimized for the sample

of this application. It may be necessary to adapt the method to your specific sample.


‐ Purity of Tris (hydroxymethyl) aminomethane used is 100.00%.

‐ Sample may be added manually using a pipette instead of using an additional dosing unit.

Literature : ‐ Ginplate Cu 406, ( http://www.growel.com/tds/796.pdf), a

trademark of Grauer & Weil India Ltd, www.growel.com ‐ Mettler – Toledo Application M064 and M003

Sample Electroless copper bath, 5 mL

Compound Sodium Hydroxide (NaOH), M = 40.00 g/moL, z = 1 Formaldehyde (HCHO), M = 30.03 g/moL, z =1

Chemicals Deionized water, 50 mL, 1 mol/L Na2SO3 (pH = 10.5), 10 mL

Titrant Hydrochloric acid, HCl c(HCl) = 0.1 mol/L

Standard Tris (hydroxymethyl) aminomethane, (THAM), 50-100 mg

Indication DGi111-Sc Combined pH glass electrode

Chemistry HCl + NaOH → NaCl + H2O HCHO + Na2SO3 + H2O → CH2OH•SO3Na + NaOH

Calculation R1 = E, pH (Dil. sample) R2 = Q*C/m*d, g/L (NaOH content) R3 = H[Nominal value of NaOH] – (Q*C/m*d), g/L (Correction for NaOH) R4 = Q*C/m*d, g/L (Formaldehyde content) R5 = H[Nominal value of formaldehyde] – (Q*C/m*d), g/L (Correction for formaldehyde) C = M/z Q = Titrant consumption in mmol. M = Molar mass of sample in g. z = Equivalent number of sample z=1 d = density of sample in g/L. m = mass of sample in mL

Waste disposal

Copper solutions: If necessary, neutralize the solution before final disposal as special waste.

Author, Version

Ruby Das, IMSG AnaChem, V 2.0 Revised: C. De Caro, MSG AnaChem




Instruments ‐ Titration Excellence T90 (Other Titrators: depending on instrument type, manual operation and method changes are necessary)


Accessories ‐ 3 x Additional dosing unit (MT-51109030) ‐ 1 x 20 mL DV1020 glass burette (MT-51107502) ‐ 2 x 10 mL DV1010 glass burette (MT-51107501) ‐ 1 x 5 mL DV 1005 glass burette (MT-51107500) ‐ 100 mL Propylene titration beakers (MT-00101974) ‐ LabX® pro titration software

Results All results Method-ID FCA Sample 5 mL (1/6) Dil.sample 12.3 pH NaOH 16.30 g/L Formaldehyde 13.25 g/L Sample 5 mL (2/6) Dil.sample 12.3 pH NaOH 16.28 g/L Formaldehyde 13.24 g/L Sample 5 mL (3/6) Dil.sample 12.3 pH NaOH 16.30 g/L Formaldehyde 13.15 g/L Sample 5 mL (4/6) Dil.sample 12.3 pH NaOH 16.28 g/L Formaldehyde 13.01 g/L Sample 5 mL (5/6) Dil.sample 12.3 pH NaOH 16.26 g/L Formaldehyde 12.91 g/L Sample 5 mL (6/6) Dil.sample 12.3 pH NaOH 16.23 g/L Formaldehyde 13.02 g/L Statistics Method-ID Cu R1 Dil.Sample Samples 6 Mean 12.3 s 0.0 srel 0 % R2 NaOH Samples 6 Mean 16.28 g/L s 0.03 srel 0.164 % R4 Formaldehyde Samples 6 Mean 13.10 g/L s 0.14 srel 1.053 %

Titration curve: NaOH content


Table of measured values : NaOH content

Volume Increment Signal Change Time Temperature mL mL pH pH s °C 0.000 NaN 12.332 NaN 0 25.0 1.000 1.000 12.325 -0.007 1 25.0 1.001 0.001 12.317 -0.008 2 25.0 1.004 0.003 12.309 -0.008 3 25.0 1.010 0.006 12.306 -0.003 4 25.0 1.017 0.007 12.308 0.002 5 25.0 1.030 0.013 12.306 -0.002 6 25.0 1.049 0.019 12.303 -0.003 7 25.0 1.075 0.026 12.304 0.001 8 25.0 1.107 0.032 12.304 0.000 9 25.0 ----------- ------------------- ----------- ------------- ---------- ---------------------- 12.768 0.168 11.824 -0.016 84 25.0 12.935 0.167 11.820 -0.004 85 25.0 13.103 0.168 11.806 -0.014 86 25.0 13.255 0.152 11.799 -0.007 87 25.0 13.422 0.167 11.787 -0.012 88 25.0 13.590 0.168 11.777 -0.010 89 25.0 13.758 0.168 11.762 -0.015 90 25.0 ----------- -------------------- ----------- ----------- -------- --------------------- 19.885 0.168 10.617 -0.097 127 25.0 19.938 0.053 10.484 -0.133 128 25.0 19.938 0.000 10.476 -0.008 129 25.0 19.938 0.000 10.468 -0.008 130 25.0 19.938 0.000 10.457 -0.011 131 25.0 19.938 0.000 10.454 -0.003 132 25.0 19.938 0.000 10.451 -0.003 133 25.0 19.938 0.000 10.448 -0.003 134 25.0 19.938 0.000 10.447 -0.001 135 25.0 19.938 0.000 10.448 0.001 136 25.0 19.938 0.000 10.445 -0.003 137 25.0 19.938 0.000 10.445 0.000 138 25.0

Titration Curve: Formaldehyde content


Table of measured values : Formaldehyde content

Volume Increment Signal Change Time Temperature mL mL pH pH s °C 0.000 NaN 11.615 NaN 0 25.0 0.001 0.001 11.615 0.000 1 25.0 0.004 0.003 11.614 -0.001 2 25.0 0.009 0.005 11.618 0.004 3 25.0 0.017 0.008 11.612 -0.006 4 25.0 0.030 0.013 11.617 0.005 5 25.0 0.049 0.019 11.611 -0.006 6 25.0 0.074 0.025 11.608 -0.003 7 25.0 0.107 0.33 11.607 -0.001 8 25.0 0.143 0.036 11.608 0.001 9 25.0 -------------------- --------------------------- ---------------- ---------------------- ------------ ---------------------- 2.985 0.168 11.322 -0.024 30 25.0 3.153 0.168 11.304 -0.018 31 25.0 3.321 0.168 11.283 -0.021 32 25.0 3.472 0.151 11.260 -0.023 33 25.0 --------------------- ----------------------------- ------------------- -------------------- ------------ ------------------------ 5.817 0.002 10.497 -0.006 52 25.0 5.817 0.000 10.494 -0.003 53 25.0 5.817 0.000 10.494 0.000 54 25.0 5.817 0.000 10.494 0.000 55 25.0 5.817 0.000 10.487 -0.007 56 25.0 5.817 0.000 10.492 0.005 57 25.0 5.817 0.000 10.492 0.000 58 25.0 5.817 0.000 10.486 -0.006 59 25.0 5.817 0.000 10.489 0.003 60 25.0 5.817 0.000 10.489 0.003 61 25.0 5.817 0.000 10.483 -0.006 62 25.0

Comments

‐ The electrode DGi111-SC is calibrated in the range of pH 9 to 12 (see application M004) ‐ Titer determination of 0.1 mol/L HCl is done as application M003 and mean value found is 1.00031. ‐ The titrator displays warnings if upper or lower result limits are exceeded. 1. EP Titration :

Continuous endpoint titration to pH 10.5, i.e. the pH value of endpoint as indicated in the literature of the manufacturer. This titration allows the determination of the NaOH content.

2. Calculation R2: NaOH content in g/L. 3. Calculation R3: Calculation of correction for NaOH in g/L. This value is the difference between the nominal value

of NaOH and the actual result. The nominal value is indicated by the manufacturer. 4. Dispense:

10mL sodium sulfite c(Na2SO3) = 1.0mol/L is dispensed. The pH value of this reagent must first be adjusted according to the pH endpoint of the subsequent EP titration in this case pH 10.5

5. Stir: During stirring time the following reaction takes place: HCHO + Na2SO3 + H2O → CH2OH•SO3Na + NaOH

Formaldehyde (HCHO) reacts with sodium sulfite, and sodium hydroxide is formed beside CH2OH•SO3Na. 6. EP Titration : Continuous endpoint titration to pH 10.5, as indicated in the literature of the manufacturer. With this titration the

NaOH formed is titrated, and from the equivalent amount of NaOH the concentration of formaldehyde is determined.

7. Calculation R4: Calculation of the formaldehyde content in g/L. 8. Calculation R5: Calculation of correction for formaldehyde in g/L. This value is the difference between the nominal

value of formaldehyde and the actual result. The nominal value is indicated by the manufacturer.

Bath Composition: ‐ This electroless alkaline copper bath is used for the deposition of relatively thick layers of copper on printed circuit

boards. The procedure is based on the chemical reduction of (weakly) complexed copper (II) ions at activated catalytic surfaces.

‐ This type of bath usually contains copper, complexing agent or mixture of complexing agents, alkali (e.g. NaOH), formaldehyde as a reducing agent and additives.

‐ The periodic bath control by titration is necessary for optimal application of the bath. The content of copper (II) ions (see M062), of free complexing agents (see M063), of hydroxide and formaldehyde as well as the pH value (this application) are determined. Concentrations values outside the limits cause failure.


Method 001 Title Type General titration Compatible with T90 ID Cu Title NaOH and Formaldehyde . . . 002 Sample Number of IDs 1 ID 1 Copper bath Entry type Fixed volume Volume 5.0 mL Density 1.0220 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary 003 Titration stand (Rondo/TowerA) Type Rondo/TowerA Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant Cu Sample Concentration 1 Volume 5.0 mL Dosing rate 60.0 mL/min Condition No 005 Dispense (normal) [2] Titrant Water.. Concentration 100 Volume 50.0 mL Dosing rate 60.0 mL/min Condition No 006 Stir Speed 30% Duration 10 s Condition No 007 Measure (normal) [1] Sensor Type pH Sensor DGi111-SC Unit pH Temperature acquisition Temperature measurement No Stir Speed 30% Acquisition of measured values Acquisition Fix Time 30 Mean value No Condition Condition No 008 Calculation R1 Result Dil.sample Result unit pH Formula R1= E Constant C= 1 M M[None] z z[None] Decimal places 1 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 009 Titration (EP) [1] Titrant Titrant HCl Concentration 0.1 mol/L Sensor Type pH Sensor DGi111-SC Unit pH Temperature acquisition Temperature measurement No Stir Speed 30% Predispense Mode Volume Volume 1.0 mL

Wait time 0 s Control Mode Absolute Tendency Negative Endpoint value 10.5 pH Cotrol band 0.3 pH Dosing rate (max) 10 mL/min Dosing rate (min) 10 µL/min Termination At EP Yes Termination delay 10 s At Vmax 30.0 mL Max. time ∞ Accompanying stating Accompanying stating No Condition Condition No 010 Calculation R2 Result NaOH Result unit g/L Formula R2= Q1*C/m*d Constant C=M/z M M[Sodium hydroxide] z z[Sodium hydroxide] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 011 Calculation R3 Result Correction Result unit g/L Formula R3=H[Nominal value_NaOH]-

(Q1*C/m*d) Constant C=M/z M M[Sodium hydroxide] z z[Sodium hydroxide] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 012 Dispense (normal) [3] Titrant SODIUM SULFITE Concentration 1 Volume 10.0 mL Dosing rate 60.0 mL/min Condition No 013 Stir Speed 30% Duration 60 s Condition Yes Formula R2>0 014 Titration (EP) [2] Titrant Titrant HCL Concentration 0.1 mol/L Sensor Type pH Sensor DGi111-SC Unit pH Temperature acquisition Temperature measurement No Stir Speed 30% Predispense Mode None Wait time 0 Control Mode Absolute Tendency Negative Endpoint value 10.5 pH Cotrol band 0.2 pH Dosing rate (max) 10 mL/min Dosing rate (min) 10 µL/min Termination At EP Yes Termination delay 10 s At Vmax 30.0 mL Max. time ∞


Accompanying stating Accompanying stating No Condition Condition Yes Formula R2>0 015 Calculation R4 Result Formaldehyde Result unit g/L Formula R4=Q[2]*C*H[Factor for 37%

formaldehyde]/m*d Constant C=M/z M M[Formaldehyde] z z[Formaldehyde] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition Yes Formula R2>0 016 Calculation R5 Result Correction Result unit g/L Formula R5=H[Nominal value

Formaldehyde]-(Q[2]*C*H[Factor for 37% formaldehyde]/m*d

Constant C=M/z M M[Formaldehyde] z z[Formaldehyde] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition Yes Formula R2>0 017 Instruction Instruction Sodium hydroxide content too

high…PLEASE CORRECT Mode Confirmation Print Yes LabX command No Condition Yes Formula R2>H[Upper limit for NaOH] 018 Instruction Instruction Sodium hydroxide content too

low…PLEASE CORRECT Mode Confirmation Print Yes LabX command No Condition Yes Formula R2<H[Lower limit for NaOH] 019 Instruction Instruction Formaldehyde content too

high…PLEASE CORRECT Mode Confirmation Print Yes LabX command No Condition Yes Formula R4>H[Upper limit for

Formaldehyde] 020 Instruction Instruction Formaldehyde content too

low…PLEASE CORRECT Mode Confirmation Print Yes LabX command No Condition Yes Formula R4<H[Upper limit for

Formaldehyde] 021 Rinse Auxillary reagent WATER Rinse cycles 1 Vol.per cycle 10 mL Position Current position Drain No Condition No

022 Condition Type Fix Interval 1 Position Conditioning beaker Time 10 s Speed 30 % Condition No 023 End of sample



Electroless Nickel Bath: Determination of Sodium Hypophosphite Method for determination of sodium hypophosphite content in electroless nickel bath by iodometric back titration.

Preparation and Procedures CAUTION - Use safety goggles, a lab coat and wear gloves. If

possible, work in a fume hood. - Ensure accurate cleaning of sensor is sufficient after

each titration.

Sample handling (Electroless nickel bath) Add 6mL of Ginplate Ni 418-A and 9 mL of Ginplate Ni 418-B in 100mL volumetric flask and make up the volume with deionized water. Shake it properly and then use it as sample.

Sample titration (Method 065a) - Take 3 mL of Nickel bath sample in 100 mL titration

beaker with graduated pipette. Add 50 mL sulfuric acid with 50 mL glass cylinder.

- Add 20 mL ½ I2 with the help of external dosing unit. After the addition of iodine immediately cover the sample beaker tightly with a lid. Keep the beaker in dark (60 min) for oxidation reaction.

- Place the oxidized sample beaker on sample changer - Titrate with 0.1mol/L Na2S2O3. - After completion of each sample, electrode, stirrer

and titration tubes will be rinsed by deionized water by means of membrane pump.

- Electrode is cleaned first with water in condition beaker placed on sample changer after each sample.

Back value (Method 065b) - Perform back value similar to sample determination

except the addition of sample and same precautious has to be taken as that of sample.

- The back value is determined and stored as B[Back Value]

Remarks

‐ Prior to use, adjust the automated titration stand by turning the small knob on the housing at 7 for rinsing and conditioning.

‐ The setting of the automated titration stand allows rinsing of 2 secs and a conditioning of 30 secs the electrode is crucial to achieve accurate and precise results.

‐ The application method has been developed for the mentioned sample. It may be necessary to optimize the method for your sample.

‐ Purity of potassium iodate used is 99.5%.

‐ Literature: Mettler-Toledo Application M065 and M009 GINPLATE Ni 418 (http://www.growel.com/tds/563.pdf)

Sample Electroless nickel bath, 3 mL

Compound Sodium hypophosphite (NaH2PO2) M = 87.97 g/mol, z = 2 Sodium hypophosphite monohydrate (NaH2PO2.H2O) M = 105.99 g/mol, z = 2

Chemicals 20% Sulfuric acid 50mL, 1 g Potassium iodide, 0.1M HCl 50 mL, 0.1 mol/L ½ I2 20 mL.

Titrant Sodium thiosulfate, Na2S2O3 c( Na2S2O3)=0.1 mol/L

Standard Potassium iodate, KIO3

20-30 mg

Indication DMi140-SC Combined platinum ring electrode

Chemistry I2 + H2PO2- + H2O 2I- +

HPO32- + 3H+

2Na2S2O3 + I2 → Na2S4O6 + 2NaI

Calculation R1 = (B – Q) *C/m*d, g/L R2 = (B – Q) *C/m*d, g/L R3 = [H-(B – Q)]*C/m*d, g/L B = Back value H = Nominal value C = M/z Q = Titrant consumption in mmol. m = mass of the sample in mL d = Density of the sample M =Molar mass of sample in g. z = Equivalent number of sample

Waste disposal

Nickel solutions: If necessary, neutralize the solution before final disposal as special waste.

Author, Version

Geeta Naik, IMSG AnaChem, V2.0 Revised: C. De Caro, MSG AnaChem




‐ XP205 Balance

Accessories ‐ Rondolino Sample Changer (MT-51108500) ‐ PP Titration beakers 100 mL (MT-00101974) ‐ Spatula ‐ Lab X® pro titration software ‐ 1 x 20 mL DV1020 glass burette (MT-51107502)

Results All results Method-ID Sodiumhypophosphite Sample 3 mL (1/6) R1 (NaH2PO2.H2O) 23.17 g/L R2 (NaH2PO2.H2O) 27.92 g/L R3 (Correction) 1.08 g/L Sample 3 mL (2/6) R1 (NaH2PO2.H2O) 23.21 g/L R2 (NaH2PO2.H2O) 27.96 g/L R3 (Correction) 1.04 g/L Sample 3 mL (3/6) R1 (NaH2PO2.H2O) 23.17 g/L R2 (NaH2PO2.H2O) 27.91 g/L R3 (Correction) 1.09 g/L Sample 3 mL (4/6) R1 (NaH2PO2.H2O) 23.11 g/L R2 (NaH2PO2.H2O) 27.85 g/L R3 (Correction) 1.15 g/L Sample 3 mL (5/6) R1 (NaH2PO2.H2O) 23.14 g/L R2 (NaH2PO2.H2O) 27.87 g/L R3 (Correction) 1.13 g/L Sample 3 mL (6/6) R1 (NaH2PO2.H2O) 23.15 g/L R2 (NaH2PO2.H2O) 27.89 g/L R3 (Correction) 1.11 g/L Statistics Method-ID Sodiumhypophosphite R2 NaH2PO2.H2O Samples 6 Mean 27.90 s 0.04 srel 0.140 %

Titration curve


Table of measured values Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C 0.000 NaN 286.1 NaN NaN 0 25.0

0.050 0.050 286.4 0.3 NaN 2 25.0 0.100 0.050 285.9 -0.5 NaN 4 25.0 0.200 0.100 286.4 0.5 NaN 7 25.0 0.300 0.100 285.7 -0.7 NaN 9 25.0 0.400 0.100 285.6 -0.1 -2.05 12 25.0 0.500 0.100 286.0 0.4 -1.50 14 25.0 0.600 0.100 284.9 -1.1 -2.11 16 25.0 0.700 0.100 285.6 0.7 -1.86 18 25.0 0.800 0.100 284.7 -0.9 -2.00 21 25.0 ---------- ------------------- ----------- ------------- --------------- --------- ----------------------- 3.800 0.100 267.8 -1.8 -14.68 93 25.0 3.900 0.100 267.0 -0.8 -15.98 96 25.0 4.000 0.100 264.4 -2.6 -18.34 99 25.0 4.100 0.100 262.8 -1.6 -19.32 102 25.0 4.200 0.100 259.8 -3.0 -19.78 106 25.0 4.300 0.100 254.9 -4.9 -59.23 108 25.0 4.400 0.100 248.8 -6.1 -145.04 111 25.0 4.500 0.100 238.4 -10.4 -223.79 113 25.0 4.560 0.060 219.5 -18.9 -268.61 120 25.0


Comments

‐ This electroless nickel bath is used for chemical nickel deposition on printed circuit boards. It consists of nickel salts, sodium hypophosphite, buffering compounds, stabilizers, accelerators, wetting and complexing agents. Decomposition products are formed during use of the bath.

‐ Titer determination of 0.1 mol/L Na2S2O3 is done as application M009 and mean value found is 0.99507. The mean value of the titer is automatically stored as part of the setup by the function TITER.

‐ Standardization of Na2S2O3: Weigh about 25 mg of potassium iodate, dissolve it in 50 mL 0.1M HCl, add 1 g KI immediate before titration and titrate with 0.1 mol/L Na2S2O3.

‐ The mean back value of a series of three samples is automatically stored as auxillary value or back value B and can therefore by applied by method 065a for determination of nickel.

‐ The storage of the mean value only occurs if it is comprised between the limits 1.5 and 2.5 mmol which assure an adequate concentration.

‐ The shelf life of the iodine solution is limited. We recommend performing back value method before each nickel content determination.

‐ The titrator displays warnings if upper or lower result limits are exceeded. The upper or lower result limits are saved as nominal values and is given in the auxillary value H[Nominal Value for NaH2PO3] etc.

‐ Oxidation is carried out at room temperature in the dark. Cover the beaker to prevent loss of iodine, the reaction requires 60 minutes to complete.


Method 065a (Sample titration) and Method 065b (Back value) 001 Title Type General titration Compatible with T90 ID Sodiumhypophosphite Title Determination of NaH2PO3 low . . . 002 Sample Number of IDs 1 ID 1 ___ Entry type Fixed volume Volume 3 mL Density 1.04 g/mL Correction factor 1.0 Temperature 25.0°C 003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1 004 Stir Speed 40% Duration 5 s Condition No 005 Titration (EQP) [1] Titrant Titrant Na2S2O3 Concentration 0.1 mol/L Sensor Type mV Sensor DM140-SC Unit mV Temperature acquisition Temperature measurement No Stir Speed 40% Predispense Mode None Wait time 0 s Control Control User Titrant addition Dynamic dE (set value) 8 mV dV (min) 0.05 mL dV (max) 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 2 s t (min) 2 s t (max) 12 s Evaluation and recognition Procedure Standard Threshold 100 Tendency Negative Ranges 0 Add. EQP criteria No Termination At Vmax 20 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No 006 Calculation R1 Result NaH2PO3

Result unit g/L Formula R1=(B[Back Value]-Q)*C/m*d Constant C=M/z M M[NaH2PO3] z z[NaH2PO3] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 007 Calculation R2 Result NaH2PO3.H2O Result unit g/L Formula R2=(B[Back Value]-Q)*C/m*d Constant C=M/z M M[NaH2PO3.H2O]

z z[NaH2PO3.H2O] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 008 Calculation R3 Result Correction Result unit g/L Formula R3=H[Nominal Value for

NaH2PO3]-((B[Back Value]-Q)*C/m*d)

Constant C=M/z M M[NaH2PO3.H2O] Z z[NaH2PO3.H2O] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 009 Instruction Instruction Sodium hypophosphite

monohydrate content too high Mode Confirmation Print Yes LabX command No Condition Yes Formula R2>H[Upper limit of NaH2PO3] 010 Instruction Instruction Sodium hypophosphite

monohydrate content too low Mode Confirmation Print Yes LabX command No Condition Yes Formula R2<[Lower limit of NaH2PO3] 011 End of sample


001 Title Type General titration Compatible with T50/T70/T90 ID BackValue Title Back Value . . . 002 Sample Number of IDs 1 ID 1 ---- Entry type Fixed volume Volume 20.0 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25 °C 003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1 004 Stir Speed 30 % Duration 10 s Condition No 005 Titration (EQP) [1] Titrant Titrant Na2S2O3 Concentration 0.1 mol/L Sensor Type mV Sensor DM140-SC Unit mV Temperature acquisition Temperature measurement No Stir Speed 40% Predispense Mode Volume Volume 15 mL Wait time 0 s Control Control User Titrant addition Dynamic dE (set value) 4 mV dV (min) 0.1 mL dV (max) 0.5 mL Mode Equilibrium controlled dE 1.0 mV dt 3 s t (min) 3 s t (max) 30 s Evaluation and recognition Procedure Standard Threshold 150 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax 30 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria Yes Accompanying stating Accompanying stating No Condition Condition No 006 Calculation R1 Result Consumption

Result unit mmol Formula R1=Q Constant C=1 M M[None] z z[None] Decimal places 4 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 007 End of sample

008 Blank Name Back Value Value B = Mean[R1] Unit mmol Limits No Condition No 009 Calculation R2 Result Mean Back Value Result unit mmol Formula R2=Mean[R1] Constant C = 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Send to buffer No Condition No



Electroless Nickel Bath: Determination of Nickel Method for determination of nickel content in electroless nickel bath.

Preparation and Procedures CAUTION ‐ Use safety goggles, a lab coat and wear gloves.

If possible, work in a fume hood. ‐ Ensure accurate cleaning of sensor is sufficient

after each titration.

Sample Preparation: ‐ Electroless nickel bath : Pipette 20 mL

Ginplate Ni 426-A and 20 mL Ginplate Ni 426-B in 200 mL volumetric flask and dilute it upto the mark with deionized water.

Sample titration: ‐ Add 0.25 g murexide trituration with NaCl

(1:500) in the beaker placed on sample changer. ‐ Dispense 5 mL sample from dosing unit. ‐ Add 50 mL of deionized water from dosing unit. ‐ Add 10 mL of buffer pH10 from dosing unit. ‐ Titrate with 0.1mol/L EDTA. ‐ After completion of each sample sensor, stirrer

and titration tubes are rinsed by deionized water by means of membrane pump.

‐ Sensor is cleaned with deion. water in the conditioning beaker placed on sample changer after each sample.

Remarks

‐ Prior to use , adjust the output signal of the DP5 PhototrodeTM to approx. 1000 mV in deion.water before starting titration (100% transmission) by turning the small knob on the housing.

‐ Rinsing and conditioning of the Phototrode is crucial to achieve accurate and precise results.

‐ Avoid formation of bubbles during titration by low speed rate of stirrer, as they disturb photometric indication.


‐ Sample may be added manually using a pipette instead of using an additional dosing unit.

Literature : ‐ Ginplate NI 426, ( http://www.growel.com/tds/549.pdf), a

trademark of Grauer & Weil India Ltd, www.growel.com ‐ Mettler-Toledo Application M066 and M007

Sample Electroless nickel bath, 5 mL

Compound Nickel, Ni M= 58.69 g/mol, z = 1

Chemicals Deionized water, 50 mL Indicator : 0.2 g Murexide trituration with NaCl (1 : 500). Buffer pH10, 10 mL

Titrant Ethylenediaminetetraacetic acid disodium, C10H14N2Na2O8•2H2O c(EDTA- Na2) = 0.1 mol/L

Standard Zinc Sulfate, ZnSO4

c( ZnSO4) = 0.1 mol/L

Indication DP5 PhototrodeTM (555 nm) (Yellow to blue-violet)

Chemistry Ni2+ + Murexide- → Ni-Murexide+

Ni-Murexide+ + EDTA4-→ Ni-EDTA2- + Murexide-

Calculation R = Q*C/m*d, g/L Q = Titrant consumption in mmol. C = M/z. M = Molar mass of sample in g. z = Equivalent no. sample, z=1 d = density of sample in g/mL. m = mass of sample in mL.

Waste disposal

Nickel solutions : If necessary, neutralize the solution before final disposal as special waste.

Author, Version

Ruby Das, IMSG AnaChem, V2.0 Revised: C. De Caro, MSGAnaChem




Instruments ‐ Titration Excellence T50/T70/T90 (Other Titrators: depending on instrument type, manual operation and method changes are necessary)


Accessories ‐ 3 x Additional dosing unit (MT-51109030) ‐ 1 x 20 mL DV1020 glass burette (MT-51107502) ‐ 2 x 10 mL DV1010 glass burette (MT-51107501) ‐ 1 x 5 mL DV 1005 glass burette (MT-51107500) ‐ 100 mL Propylene titration beakers (MT-00101974) ®

Results All results Method-ID Nickel determination Sample 5 mL (1/6) R1 (Nickel) 5.44 g/L Sample 5 mL (2/6) R2 (Nickel) 5.44 g/L Sample 5 mL (3/6) R3 (Nickel) 5.45 g/L Sample 5 mL (4/6) R4 (Nickel) 5.43 g/L Sample 5 mL (5/6) R5 (Nickel) 5.43 g/L Sample 5 mL (6/6) R6 (Nickel) 5.44 g/L Statistics Method-ID Nickel determination R1 Nickel Samples 6 Mean 5.44 s 0.01 srel 0.138%

Titration curve


Table of measured values Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C 0.000 NaN 757.2 NaN NaN 0 25.0 0.5715 0.5715 748.2 -9.0 NaN 5 25.0 0.8570 0.2855 739.0 -9.2 NaN 13 25.0 1.0000 0.1430 738.4 -0.6 NaN 16 25.0 1.1000 0.1000 734.0 -4.4 NaN 20 25.0 1.2000 0.1000 732.1 -1.9 -25.96 24 25.0 1.3000 0.1000 729.6 -2.5 -24.64 28 25.0 1.4000 0.1000 727.1 -2.5 -26.16 32 25.0 1.5000 0.1000 723.3 -3.8 -24.72 37 25.0 1.6000 0.1000 721.7 -1.6 -24.40 42 25.0 1.7000 0.1000 720.6 -1.1 -23.28 44 25.0 1.8000 0.1000 716.7 -3.9 -24.36 50 25.0 1.9000 0.1000 713.5 -3.2 -28.28 55 25.0 2.0000 0.1000 713.0 -0.5 -29.78 58 25.0 2.1000 0.1000 708.5 -4.5 -30.43 62 25.0 ------------ ------------------- --------- ----------- --------------- ------ ----------- 4.3440 0.0500 518.0 -17.4 -358.17 184 25.0 4.3940 0.0500 499.4 -18.6 -421.44 190 25.0 4.4440 0.0500 476.6 -22.8 -538.07 196 25.0 4.4940 0.0500 446.3 -30.3 -658.13 202 25.0 EQP1 4.540268 NaN 420.7 NaN -659.56 NaN NaN 4.5440 0.0500 418.6 -27.7 -657.52 210 25.0 4.5940 0.0500 379.1 -39.5 -544.67 218 25.0 4.6440 0.0500 339.4 -39.7 -393.50 230 25.0 4.6940 0.0500 322.0 -17.4 -269.40 239 25.0 4.7600 0.6600 320.1 -1.9 -148.20 243 25.0 4.8600 0.1000 319.3 -0.8 NaN 245 25.0 4.9600 0.1000 319.6 0.3 NaN 248 25.0 5.0600 0.1000 320.4 0.8 NaN 250 25.0 5.1600 0.1000 321.2 0.8 NaN 253 25.0 5.2600 0.1000 321.9 0.7 NaN 255 25.0

Comments

‐ Titer determination of 0.1 mol/L EDTA-Na2 is done as per the Mettler –Toledo method application M007 and mean value found is 0.99163.

‐ The mean value of the titer is automatically stored as part of the setup by the function TITER. ‐ The buffer pH 10 is prepared by dissolving 64 g NH4Cl in 600mL 25% Ammonia solution and diluting it

upto the mark with deionized water in a 1L volumetric flask.. ‐ The shape of the titration curve is somewhat affected by the concentration of the indicator. The results,

however do not differ significantly ( tested range: 25-500 mg of Murexide trituration with NaCl(1 :500). ‐ Add the indicator before starting analysis. Keep sample free of air bubbles during titration. Air bubbles

and undissolved impurities affect the photometric indication. ‐ Due to the steep signal change, an EQP titration with fixed increments is used. The low threshold

value allows for different amounts of indicator. Principle : ‐ Nickel ions forms yellow complex with murexide in alkaline solution: Ni2+ + Murexide- → Ni-Murexide+

‐ By adding EDTA , Ni forms a more stable complex with EDTA:

Ni-Murexide+ + EDTA4- → Ni-EDTA2- + Murexide- At the equivalence point, all Ni ions have been complexed by EDTA and murexide is free in the alkaline solution. There is a colour change from yellow to blue-violet.


Method 001 Title Type General titration Compatible with T50 / T70 / T90 ID Nickeldetermination Title Ni determination . . . 002 Sample Number of IDs 1 ID 1 Nickel Entry type Fixed volume Volume 5.0 mL Density 1.03 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary 003 Titration stand (Rondo/TowerA) Type Rondo/TowerA Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant NI SAMPLE Concentration 1 Volume 5.0 mL Dosing rate 60.0 mL/min Condition No 005 Dispense (normal) [2] Titrant Water.. Concentration 1 Volume 50.0 mL Dosing rate 60.0 mL/min Condition No 006 Dispense (normal) [3] Titrant BUFFER 10PH Concentration 1 Volume 10.0 mL Dosing rate 60.0 mL/min Condition No 007 Stir Speed 10% Duration 60 s Condition No 008 Titration (EQP) [1] Titrant Titrant EDTA(0.1M) Concentration 0.1 mol/L Sensor Type Phototrode Sensor DP5 Unit mV Temperature acquisition Temperature measurement No Stir Speed 10% Predispense Mode Volume Volume 1.0 Wait time 0 s Control Control User Titrant addition Dynamic dE (set value) 10 mV dV (min) 0.05 mL dV (max) 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 2 s t (min) 2 s t (max) 12 s Evaluation and recognition Procedure Standard Threshold 200.0 mV/mL Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax 10.0 mL 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 009 Calculation R1 Result Ni content Result unit g/L Formula R1= Q*C/m*d Constant C=M/z M M[Nickel] z z[Nickel] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 010 Rinse Auxillary reagent WATER Rinse cycles 1 Vol.per cycle 10 mL Position Current position Drain No Condition No 011 Condition Type Fix Interval 1 Position Conditioning beaker Time 20 s Speed 10 % Condition No 012 End of sample



Electroless Nickel Bath: Determination of Sodium Orthophosphite Method for determination of Sodium orthophosphite content in electroless nickel bath by iodometric back titration.

Preparation and Procedures CAUTION ‐ Use safety goggles, a lab coat and wear gloves. If

possible, work in a fume hood. ‐ Ensure accurate cleaning of sensor is sufficient after

each titration. Sample handling Electroless Nickel bath: Take 6 mL of Ginplate Ni 418-A and 9 mL of Ginplate Ni 418-B in 100 mL volumetric flask and make up the volume with deionized water. Shake it properly and then use it as sample.

Sample titration ‐ Take 0.5 mL of electroless nickel bath sample in 100

mL titration beaker with a 1 mL pipette. ‐ Add 5 % sodium bicarbonate 20 mL in 100 mL

titration beaker with a 25 mL glass cylinder ‐ Add 20 mL ½ I2 with help of external dosing unit. After

the addition of iodine immediately cover the beaker to avoid loss of released iodine.

‐ Keep it in dark for 30 min for oxidation reaction ‐ Place the oxidized sample on sample. ‐ Immediately before titration the sample is acidified by

adding 2 mol/L acetic acid 20 mL with additional dosing unit.

‐ Titrate with 0.1mol/L Na2S2O3 ‐ After completion of each sample, electrode, stirrer

and titration tubes will be rinsed by deionized water by means of membrane pump

‐ Electrode is cleaned first with water in condition beaker placed on sample changer after each sample.

Blank (or Back) value ‐ Perform blank similar to sample determination

except the addition of sample and same precautious has to be taken as that of sample..

‐ The back value is determined and stored as B[Back Value ophosphite]

Remarks

‐ Prior to use, adjust automated titration stand by turning the small knob on the housing of the stand at pos. 7 for electrode conditioning.

‐ The setting allows for rinsing (2 s) and conditioning (30 s) of the electrode. This is crucial for accurate and precise results.

‐ The application method has been developed for the mentioned sample. It may be necessary to optimize the method for your sample.

‐ Purity of potassium iodate used is 99.5%. ‐ Literature:

Mettler-Toledo Application M067 and M009. GINPLATE Ni 418 (www.growel.com/tds/563.pdf )

Sample Electroless nickel bath, 0.5 mL

Compound Disodium hydrogen phosphite (Na2HPO3) M = 125.96 g/mol, z = 2 Sodium dihydrogenphosphite (NaH2PO2) M = 105.99 g/mol, z = 2 Phosphorous acid (H3PO3) M = 81.99 g/mol, z = 2

Chemicals 20mL 2 M Acetic acid (CH3COOH), 1 g Potassium iodide (KI), 20 mL 5% Sodium hydrogen carbonate (NaHCO3) 20 mL 0.1 M ½ I2 Iodine , 50 mL 0.1 M HCl

Titrant Sodium thiosulfate, Na2S2O3 c(Na2S2O3) = 0.1 mol/L

Standard Potassium iodate, KIO3

20-30 mg

Indication DMi140-SC Combined platinum ring electrode

Chemistry I2 + HPO32- + 3OH- →

2I- + PO43- + 2H2O

2Na2S2O3 + I2 → Na2S4O6 + 2NaI

Calculation R1 = (B – Q) *C/m*d, g/L R2 = (B – Q) *C/m*d, g/L R3 = (B – Q) *C/m*d, g/L B = Back value C = M/z Q = Titrant consumption in mmol. m = mass of the sample in mL d = Density in g/mL M =Molar mass of sample in g. z = Equivalent number of sample

Waste disposal

Nickel solutions: If necessary, neutralize the solution before final disposal as special waste.

Author, Version

Geeta Naik, IMSG AnaChem, V 2.0 Revised: C. De Caro, MSG AnaChem




‐ XP205 Balance

Accessories ‐ 1 x 20 mL DV1020 glass burette (MT-51107502) ‐ 1 x Additional dosing unit (MT-51109030 ‐ PP Titration beakers 100 mL (MT-00101974) ‐ Rondolino Automate Titration Stand (MT-51108500) ‐ LabX® pro titration software ‐ Spatula

Results All results Method-ID Orthophosphite Sample 0.5 mL (1/6) R1 (Na2HPO3) 9.90 g/L R2 (NaH2PO3) 8.18 g/L R3 (H3PO3) 6.45 g/L Sample 0.5 mL (2/6) R1 (Na2HPO3) 9.97 g/L R2 (NaH2PO3) 8.23 g/L R3 (H3PO3) 6.49 g/L Sample 0.5 mL (3/6) R1 (Na2HPO3) 9.92 g/L R2 (NaH2PO3) 8.19 g/L R3 (H3PO3) 6.46 g/L Sample 0.5 mL (4/6) R1 (Na2HPO3) 10.17 g/L R2 (NaH2PO3) 8.40 g/L R3 (H3PO3) 6.62 g/L Sample 0.5 mL (5/6) R1 (Na2HPO3) 10.25 g/L R2 (NaH2PO3) 8.46 g/L R3 (H3PO3) 6.67 g/L Sample 0.5 mL (6/6) R1 (Na2HPO3) 10.38 g/L R2 (NaH2PO3) 8.57 g/L R3 (H3PO3) 6.76 g/L Statistics Method-ID orthophosphite R1 Na2HPO3 Samples 6 Mean 10.10 s 0.20 srel 1.956 %

Titration curve


Table of measured values Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C 0.000 NaN 407.5 NaN NaN 0 25.0

8.571 8.571 398.9 -8.6 NaN 12 25.0 12.857 4.286 391.0 -7.9 NaN 20 25.0 15.000 2.143 385.1 -5.9 NaN 25 25.0 15.100 0.100 385.5 0.4 NaN 59 25.0 15.200 0.100 385.0 -0.5 -3.01 62 25.0 15.300 0.100 384.5 -0.5 -3.26 66 25.0 15.400 0.100 384.0 -0.5 -3.14 69 25.0 15.500 0.100 384.1 0.1 -3.59 72 25.0 15.600 0.100 383.7 -0.4 -3.16 76 25.0 ---------- ------------------- ----------- ------------- --------------- --------- ----------------------- 18.900 0.100 358.7 -1.6 -17.69 189 25.0 19.000 0.100 357.1 -1.6 -21.10 193 25.0 19.100 0.100 354.1 -3.0 -26.09 197 25.0 19.200 0.100 351.3 -2.8 -32.66 200 25.0 19.300 0.100 347.6 -3.7 -43.74 204 25.0 19.400 0.100 342.5 -5.1 -99.50 207 25.0 19.461 0.061 338.3 -4.2 -154.43 211 25.0 19.511 0.050 333.4 -4.9 -235.82 214 25.0 19.561 0.050 324.6 -8.8 -305.97 218 25.0


Comments

• This electroless nickel bath is used for chemical nickel deposition on printed circuit boards. It consists of nickel salts, sodium hypophosphite, buffering compounds, stabilizers, accelerators, wetting and complexing agents. Decomposition products are formed during use of the bath.

• Titer determination of 0.1mol/L Na2S2O3 is done as per the Mettler-Toledo method application M009 and mean value found is 0.99896. The mean value of the titer is automatically stored as part of the setup by the function TITER.

• Standardization of Na2S2O3: Weigh about 25 mg of potassium iodate, dissolve it in 50 mL mol/L HCl add 1 g KI immediate before titration and titrate with 0.1 mol/L Na2S2O3

• The mean value of a series of three samples is automatically stored as auxillary value or back value B and can therefore applied by method content determination for determination of nickel.

• The storage of the mean value only occurs if it is comprised between the limits 1.5 and 2.5 mmol which assure an adequate concentration.

• The shelf life of the iodine solution is limited. We recommend performing back value method before each nickel content determination.

• If the orthophosphite concentration exceeds the limit given as per the sample e.g. 20 g/L, an instruction is displayed.

• Oxidation is carried out at room temperature in the dark. Cover the beaker to prevent loss of iodine, the reaction requires 30 minutes to complete.


Method 001 Title Type General titration Compatible with T90 ID orthophosphite Title EQP . . . 002 Sample Number of IDs 1 ID 1 -- Entry type Fixed volume Volume 0.5 mL Density 1.03 g/mL Correction factor 1.0 Temperature 25.0°C 003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1 004 Dispense (normal) [1] Titrant Acetic acid Concentration 2 mol/L Volume 20 mL Dosing rate 60.0 mL/min Condition No 005 Stir Speed 30% Duration 10 s Condition No 006 Titration (EQP) [1] Titrant Titrant Na2S2O3 Concentration 0.1 mol/L Sensor Type mV Sensor DM140-SC Unit mV Temperature acquisition Temperature measurement No Stir Speed 30% Predispense Mode Volume Volume 15 mL Wait time 30 s Control Control User Titrant addition Dynamic dE (set value) 4.0 mV dV (min) 0.05 mL dV (max) 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 3 s t (min) 3 s t (max) 30 s Evaluation and recognition Procedure Standard Threshold 200 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax 30 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

007 Calculation R1 Result Na2HPO3

Result unit g/L Formula R1=(B[Back Value]-Q)*C/m*d Constant C=M/z M M[Di Sodium hydrogen

phosphite] z z[Di Sodium hydrogen

phosphite] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 008 Calculation R2 Result NaH2PO3 Result unit g/L Formula R2=(B[Back Value]-Q)*C/m*d Constant C=M/z M M[Sodium dihydrogen

phosphite] z z[Sodium dihydrogen

phosphite] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 009 Calculation R3 Result H3PO3

Result unit g/L Formula R3=(B[Back Value]-Q)*C/m*d Constant C=M/z M M[Phosphoric acid] Z z[Phosphoric acid] Decimal places 2 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 010 Instruction Instruction Check concentration of

phosphite Mode Confirmation Print Yes LabX command No Condition Yes Formula R2>H[Nominal value for

NaH2PO3(o)] 011 End of sample


001 Title Type General titration Compatible with T50/T70/T90 ID BackValueOphosphite Title Back Value of Orthophosphite . . . 002 Sample Number of IDs 1 ID 1 -- Entry type Fixed volume Volume 20 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C 003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1 004 Dispense (normal) [1] Titrant Acetic acid Concentration 2 mol/L Volume 20 mL Dosing rate 60.0 mL/min Condition No 005 Stir Speed 30% Duration 10 s Condition No 006 Titration (EQP) [1] Titrant Titrant Na2S2O3 Concentration 0.1 mol/L Sensor Type mV Sensor DM140-SC Unit mV Temperature acquisition Temperature measurement No Stir Speed 30% Predispense Mode Volume Volume 15 mL Wait time 10 s Control Control User Titrant addition Dynamic dE (set value) 0.5 mV dV (min) 0.1 mL dV (max) 1.5 mL Mode Equilibrium controlled dE 1.0 mV dt 3 s t (min) 3 s t (max) 30 s Evaluation and recognition Procedure Standard Threshold 150 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax 30 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

007 Calculation R1 Result Consumption

Result unit mmol Formula R1=Q Constant C=1 M M[None] z z[None] Decimal places 4 Result limits No Record statistics Yes Extra statistical func. No Send to buffer No Condition No 008 End of sample 009 Blank Name Back Value ophosphite Value B = Mean[R1] Unit mmol Limits No Condition No 010 Calculation R2 Result Mean Back Value Result unit mmol Formula R2=Mean[R1] Constant C = 1 M M[None] z z[None] Decimal places 4 Result limits No Record statistics Yes Send to buffer No Condition No

METTLER TOLEDO

METTLER TOLEDO Electroplating Industry

Literature

1. "Electrochemistry of semiconductors and Electronics: Processes and Devices", Eds. John McHardy and Frank Ludwig, Noyes Publications, Park Ridge, New Jersey (USA) 1992 (ISBN 0-8155-1301-1).

2. Kenneth E. Langford, Janet Parker, "Analysis of electroplating and related solutions", 4th Edition, Robert Draper Ltd, Teddington (UK), 1971 (ISBN 0-8521-8033-0).

3. Peter Wolfram Wild, "Modern Analysis for Electroplating", Hampton Hill Finishing Publications, 1974.

This application bulletin represents selected, possible application examples. These have been tested with all possible care in our lab with the analytical instrument mentioned in the bulletin. The experiments were conducted and the resulting data evaluated based on our current state of knowledge.

However, the application bulletin does not absolve you from personally testing its suitability for your intended methods, instruments and purposes. As the use and transfer of an application example are beyond our control, we cannot accept responsibility therefore.

When chemicals and solvents are used, the general safety rules and the directions of the producer must be observed.

www.mt.comFor more information

Mettler-Toledo AG, AnalyticalCH-8603 Schwerzenbach, SwitzerlandTel. +41 44 806 77 11Fax +41 44 806 72 40

Subject to technical changes© 04/2013 Mettler-Toledo AG, 724561A Market Support Group AnaChem

Selected Applications in The Electroplating Industry Periodic check and exact knowledge of the concentration in an electroplating bath are a crucial issue to achieve an efficient and optimum plating treatment.

Titration Applications Brochure No. 4 is a collection of representative methods for the concentration determination of several components in copper and nickel plating baths.

METTLER TOLEDO offers you a variety solutions for automated titration analyses in the electroplating industry.

Titration Applications Brochure 4

T50A Terminal T70 with Terminal and two additional dosing units

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