Semilux 100 Ds v05

NICKEL Version: 05
Doc.-No.: 2359
DATA SHEET
SAP-No.: 1679331
Semilux 100 IMDS-No.: 114806927

Semi-bright nickel plating process
CONTENTS
1. Process Information................................................................................................................................. 2
2. Equipment ............................................................................................................................................... 2
3. Make-Up .................................................................................................................................................. 4
4. Working Parameters ................................................................................................................................ 5
5. Maintenance ............................................................................................................................................ 6
General Data of Plating Solution ........................................................................................................ 6
Function of the Additives .................................................................................................................... 7
6. SAP No. for Make-Up and Maintenance Products .................................................................................. 9
7. Recommendations for Wastewater Treatment ...................................................................................... 10
8. Analytical Instructions ............................................................................................................................ 11
Complexometric Determination of Nickel by Titration ...................................................................... 11
Determination of Chloride by Titration .............................................................................................. 14
Determination of the Boric Acid Content by Titration ....................................................................... 16
Titrimetric Determination of Boric Acid with Glycerin Citrate Solution ("Mixed Solution")................ 18
Semilux 101 Make Up and Semilux 102 Brightener by LC .............................................................. 20
Semilux SE1 using LC-UV ............................................................................................................... 24
9. Document History .................................................................................................................................. 28
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Version: 05
Semilux 100
Semi-bright nickel plating process Doc.-No.: 2359
1. Process Information
The Semilux 100 nickel plating process produces a highly levelled, ductile, semi-bright deposit exhibiting
exceptional corrosion protection when used as the undercoat in a duplex or multi layer nickel system.
The Semilux 100 process is characterized by:
• A process that can be used on a variety of substrates as steel, brass, zinc-die castings, copper
or plastics.
• Excellent levelling and ductile deposit.
• High STEP values, 110 – 170 mV range.
• Improved corrosion protection characteristics.
• Easy conversion from other semi-bright nickel plating processes.
2. Equipment
Tanks Mild steel with hard rubber lining, PVC as well as

PVC/Polyester reinforced material or PP.
Heating Heat exchanger, heating coils or immersion heaters made of

graphite, titanium (anodic), PTFE, hard glass or porcelain.
Anodes Rolled pure nickel anodes, electrolytic nickel anodes in

titanium anode baskets.
Anode Bags Required, use of twin bags is recommended.

Made of Dynel or PP leached in a 10 % sulfuric acid solution
and then flushed with hot running water prior to use.
Filtration Continuous. Pumps and filters (recommended: plate filter)

must be made of acid-resistant materials and be able to
ensure a circulation of the electrolyte for 5 – 6 times per hour.
Filter grade: < 5 µm
Filter surface: > 10 cm²/liter bath volume.
Applicable Filter Aid Diatomaceous earth or cellulose with activated carbon.
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Air Agitation / Mechanical Agitation Mechanical as well as air agitation must be provided to
ensure high rates of deposition as well as excellent leveling.
Air agitation:
The required amount of air is about 15 – 20 m3/h per meter
cathode rod. The spargers are installed parallel to the
cathode rod and to each other; about 30 – 80 mm above the
tank bottom. Depending on the size of the tank the spargers
will be drilled with 3 mm holes at intervals of 100 mm at an
angle of 45° to the tank bottom. Each pipe has two rows of
holes set opposite to each other at intervals of 40 – 50 mm.
It is recommended to install at least two feeding pipes. The
distance of the pipes to each other is to be 150 – 250 mm
(inner diameter 20 – 40 mm). Suitable materials are PP or
PVC. To avoid contamination of the plating solution by oil
compressed air must not be used.
Mechanical agitation:
Additional cathode rod movement proved beneficial to ensure
that all areas of the parts are reached by the air stream.
Cathode rod movement should be horizontal.
stroke length double strokes/min

horizontal: 100 mm 20 – 25
vertical: 60 mm 25 – 30
Exhaust Required.
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3. Make-Up
Make-Up of 100 l Liter kg

Nickel Sulfate (NiSO4 • 6 H2O) --- 28
Nickel Chloride (NiCl2 • 6 H2O) --- 4.0
Boric Acid --- 4.5
Semilux 101 Make Up 0.3 ---
Semilux 102 Brightener 0.04* ---
Semilux SE1 0.03 ---
or
Semilux SE2 (for low hardness requirement) 0.075 ---
Wetting Agent NP-A or Nickel Additive Y-17
(with air agitation)
0.1 ---
Wetting Agent Ni 86 conc
(with mechanical agitation)
* For applications requiring deposits with better brightness and levelling the make-up concentration of Semilux 102 Brightener
could be increased to 0.06 ml per 100 l (0.6 ml/l).
The plating tank and all associated plumbing, including pumps, spargers, heaters, filters, racks, etc., should
be cleaned. A clean, off-line heated tank should be used to prepare the working plating solution.
• Dissolve the boric acid, nickel sulfate and nickel chloride in hot (70 – 80 °C) DI-water while stirring well.
Use a steel tank with a vitreous enamel lining or a stainless steel (grade 316), PP, CPVC or PVC tank
for this operation. To dissolve approx. 37 kg of the combined nickel salts and boric acid, at least 50 l
water are needed at 80 °C.
• Add 5 g/l pulverized activated carbon (low sulfur, low iron; suitable activated carbon can be purchased
from Atotech) and stir for 30 – 60 min. Turn off the agitation to allow the activated carbon to settle to the
bottom of the tank for 3 – 4 hours – preferably overnight.
• Filter the solution back into the clean working tank (Ensure that the temperature of the solution during
filtration stays above 50 °C to prevent precipitation of boric acid).
• Fill the tank to nearly the final volume with DI-water, check the operating temperature and adjust if
necessary.
• Adjust the pH as required with a 10 % (v/v) sulfuric acid.
• Dummy plate solution with steel panels (degreased, descaled and/or nickel plated) at 1.5 – 2.5 A/dm2
for 2 Ah/l. Use of agitation and filtration during this period is beneficial.
• Readjust the pH, if necessary.
• Add the required amounts of
Semilux 101 Make Up

Semilux 102 Brightener
Semilux SE1
Semilux SE2
Wetting Agent NP-A or Nickel Additive Y-17 or
Wetting Agent Ni 86 conc
and circulate for 20 minutes to assure thorough mixing. The electrolyte is now ready for use.
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4. Working Parameters
pH 4.0 (3.8 – 4.4)
Temperature 55 °C (52 – 62 °C)

Equipment requirements should be considered, e.g. tank
linings and air agitation lines, when operating at higher
temperatures.
Agitation Mechanical and / or air.
Cathode Current Density 4 A/dm² (2 – 5 A/dm²)
Anodic Current Density < 3 A/dm² in highly agitated tanks

< 1.8 A/dm² in “still” tanks
Ratio Anode : Cathode 1.5 : 1 – 2 : 1
Rectifier DC with a ripple of < 5 %
Voltage 8 – 15 V
Rate of Deposition 0.8 µm/minute at 4 A/dm²
Cathodic Current Efficiency 94 – 95 %
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5. Maintenance
General Data of Plating Solution
Nominal values On make up During operation

Nickel 72.3 g/l 68 – 80 g/l
Chloride ions 12.0 g/l 11 – 16 g/l
Boric acid 45 g/l 40 – 50 g/l
Additions of 10 g/l each of the following salts will change the inorganic bath values as follows:
Salt Nickel Chloride ions Boric Acid

10 g/l Nickel Sulfate (NiSO4 • 6 H2O) 2.2 g/l --- ---
10 g/l Nickel Chloride (NiCl2 • 6 H2O) 2.5 g/l 3.0 g/l ---
10 g/l Boric acid (H3BO3) --- --- 10.0 g/l
The pH can be adjusted with sulfuric acid (diluted to 10 % (v/v)) or – if there is a lack of chloride ions – with
hydrochloric acid (diluted at a ratio of 1 : 1).
Evaporation losses must be replenished by adding distilled or deionized water.
Nickel
The nickel content should be determined at least once a week and adjusted at regular intervals. Normally a
concentration of 68 – 80 g/l is specified, because this provides a sufficiently high metal concentration for all
purposes. If the plating job is particularly difficult (deep recesses, sharp corners, irregular shapes, etc.) or if
the current concentration required is above 4.5 – 6.5 A/l, the nickel concentration should be carried at the
higher level, the top value depends upon requirements.
Chloride
The chloride content should be determined and corrected at the same frequency suggested for nickel and
should be maintained within the limits specified. Too low chloride content will result in poor anode corrosion
and low efficiency leading to depletion of the nickel content of the solution and/or breakdown of the addition
agents. Too high chloride content reduces the ductility and increases the internal stress of the Ni deposit.
Boric Acid
The boric acid content of the solution should be determined and adjusted at least once a week. The control
and maintenance of the boric acid content of the plating solution between the specified limits is essential. At
boric acid concentrations > 50 g/l crystallization of the boric acid could take place of the solution is allowed to
cool down causing roughness of the deposit. Lack of boric acid results in a reduced cathodic efficiency which
is visible by increased gassing at the cathode.
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Function of the Additives
Consumption for 10,000 Ah

Semilux 101 Make Up mainly through drag-out (0.2 – 0.4 l)
Semilux 102 Brightener 0.7 – 2.4 l (depending on required leveling)
Semilux 103 Booster optional
Semilux SE1 depending on required STEP (0.5 – 1.0 l)
or
Semilux SE2 (for low hardness requirement) depending on required STEP 2.0 – 4.0 l
Wetting Agent NP-A or Nickel Additive Y-17 approx. 0.2 l
Wetting Agent Ni 86 conc approx. 0.2 l
Semilux 101 Make Up

Semilux 101 Make Up produces the desired deposit characteristics by functioning co-operatively with the
Semilux 102 Brightener additive. Semilux 101 Make Up acts as a hardness reducer preferably in the low
current density areas and also reduces the internal stress of the Ni-deposit.
Semilux 101 Make Up is mainly added at the time of make-up. Semilux 101 Make Up is lost mainly by
drag-out. Semilux 101 Make Up can be added directly to the plating tank without dilution. Care should be
taken to ensure uniform distribution throughout the plating tank. Normal carbon filtration (1 – 2 g/l) will not
remove a significant amount of Semilux 101 Make Up. Heavy carbon treatment (5 – 10 g/l) may remove up
to 50 % of the Semilux 101 Make Up.
Semilux 102 Brightener

The function of this addition agent is to work in conjunction with Semilux 101 Make Up to produce the
desired deposit characteristics. Generally, Semilux 102 Brightener contributes to the levelling and overall
semi-brightness. For standard POP-application, Semilux 102 Brightener concentrations between 0.4 and
0.6 ml/l are recommended. For application on metal substrates, e.g. steel, which require higher levelling,
Semilux 102 Brightener concentrations between 0.6 and 1.0 ml/l are recommended. The consumption of
Semilux 102 Brightener is approx. 0.7 – 2.4 l per 10000 Ah depending on the levelling required, drag-out,
installation conditions, etc.
Semilux 102 Brightener consumption for 10,000 Ah at varying make up concentrations

0.4 ml/l Semilux 102 Brightener 0.7 – 0.8 l
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High concentration of Semilux 102 Brightener (> 0.8 ml/l) can result in relief formation in areas of very low
local current densities. This effect can be reduced by lowering the pH, reducing the strength of air agitation
or increasing the current density. If even higher leveling is required Semilux 103 Booster should be used
instead of further additions of Semilux 102 Brightener.
Semilux 102 Brightener should be added in smaller portions to avoid large over-the-side additions that
could also cause a temporarily change of the resultant deposit. It is recommended that initially the Semilux
102 Brightener is determined once per eight hour shift to establish the consumption rate and thereafter
dosing as required. The consumption of Semilux 102 Brightener will typically be higher when inert or
auxiliary anodes are utilized. An excess of Semilux 102 Brightener in the plating solution can be removed
through electrolysis.
Semilux SE1
Semilux SE1 is used to maintain or increase the STEP (potential difference between semi-bright and bright
nickel deposits) and to improve the brightness of the deposit in medium to low current density areas.
0.1 ml/l Semilux SE1 will increase the STEP approx. by 10 – 20 mV.
Semilux SE1 retains all of the appearance and performance characteristics of Semilux 102 Brightener and
also provides the consistently high STEP (110 – 170 mV).
Semilux SE1 functions with Semilux 101 Make Up and Semilux 102 Brightener to control the brightness
and STEP of the Semilux 100 deposit in a duplex or multi layer nickel system. Excessive concentrations of
Semilux SE1 may result in reduced ductility, increased hardness and increased internal stress. Electrolysis
will reduce excessive concentrations of Semilux SE1.
Semilux SE2
Semilux SE2 is used to maintain or increase the STEP (potential difference between semi-bright and bright
nickel deposits) instead of Semilux SE1 in case a low hardness of the SB-Ni deposit is required.
0.5 ml/l Semilux SE2 will increase the STEP approx. by 10 – 20 mV.
Semilux SE2 retains all of the appearance and performance characteristics of Semilux 102 Brightener and
also provides the consistently high STEP (110 – 170 mV).
Semilux SE2 functions with Semilux 101 Make Up and Semilux 102 Brightener to control the brightness
and STEP of the Semilux 100 deposit in a duplex or multi layer nickel system. Excessive concentrations of
Semilux SE2 may result in reduced ductility, increased hardness and increased internal stress. Electrolysis
will reduce excessive concentrations of Semilux SE2.
Semilux 103 Booster

Semilux 103 Booster can be used if additional leveling is necessary.
The dosing of Semilux 103 Booster is approx. 0.5 l (0 – 2.0 l) per 10000 Ah depending on the required
leveling, drag-out, installation conditions, etc. For dosing Semilux 103 Booster can be mixed with
Semilux 102 Brightener.
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Wetting Agent NP-A, Nickel Additive Y-17 and Wetting Agent Ni 86 conc
These addition agents are wetting agents and perform their function by lowering the surface tension of the
nickel plating solution. Wetting Agent NP-A / Nickel Additive Y-17 is a low foaming type of wetting agent
and should be used in air agitated solutions. Wetting Agent Ni 86 conc. will only be required in
mechanically agitated solutions. Excessive usage of Wetting Agent NP-A / Nickel Additive Y-17 or
Wetting Agent Ni 86 conc usually indicates contamination of the plating solution and steps should be taken
to eliminate the source of contamination.
Selective Cleaning
All nickel plating solutions develop some type of inorganic and organic contamination due to drag-in,
decomposition of additives or by electrolysis. Therefore, it is recommended that all nickel plating solutions be
treated on a regular basis. The scheduling of maintenance and treatment of nickel plating baths depends on
the amount of work processed through the solution, the number of ampere-hours per volume of solution, the
amount of drag-in from previous operations, or if the bath has been idle for an extended period of time. If
insoluble auxiliary anodes are used, the solution should be treated more frequently.
6. SAP No. for Make-Up and Maintenance Products
PRODUCT SAP No.

SEMILUX 101 MAKE UP 1684775
SEMILUX 102 BRIGHTENER 1684776
SEMILUX SE1 1689064
SEMILUX 103 BOOSTER 1687266
SEMILUX SE2 1689068
NICKEL ADDITIVE Y-17 2200983
WETTING AGENT NP-A 1667582
WETTING AGENT NI 86 CONC 1421692
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7. Recommendations for Wastewater Treatment
Rinse water
Nickel can be precipitated by adjusting the rinse water pH to between 9.5 – 10. The filtered solution can
subsequently be sent to final neutralization.
Concentrates
The following options are possible when concentrated Nickel solutions must be treated.
When nickel is to be recycled, it is generally necessary to treat these nickel solutions separately from other
solutions.
The following recycling methods are typical, although others can be recommended:
• Electrowinning of nickel using an appropriated electrolytic cell.
• Treatment of nickel concentrate, or of a precipitated nickel sludge, by a specialized recycling company.
If these methods cannot be used, the nickel concentrate together with the complexing agent free
wastewaters can be treated by adjusting the pH to between 9.5 – 10. For better precipitation the
concentrates must be diluted in a ratio of 1 : 10 before sending to the wastewater treatment plant.
For better flocculation we recommend to add a flocculant (e.g. a polyacrylamide / anionic with a mol mass of
4 – 6 million). The solution is then stirred and the precipitation is allowed to settle for better filtration.
Concentrate regeneration
The available bath regeneration system using membrane anodes and adsorber type Nikotect can be
recommended. Please see the respective special data sheet for details.
Membrane anodes:
This system avoids an increasing of the Ni-content in the bath due to different current efficiencies at
the electrodes.
Adsorber:
The adsorber system using a special resin eliminates organic contaminations from the Ni-electrolyte.
This recommendation for the treatment of wastewater is in accordance with the Regulation
on requirements for the discharge of wastewater into water (Allgemeine
Abwasserverordnung, AbwV) and was issued on the basis of the limits provided in Annex
40 of the AbwV "Metal Handling and Metal Processing".
Be sure to observe all local regulations concerning the limiting values of pollutants
including the general regulations on dangerous materials!
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8. Analytical Instructions
Version: 04
Complexometric Determination of Nickel by Titration
Doc.-No.: A0000364-04
Principle: Complexometric titration
Reagents for manual titration:
• 0.1M Na2-EDTA volumetric standard

• 25 % Ammonia solution
• Murexide indicator triturate (1 : 100 with sodium chloride)
Reagents for titroprocessor:
• 0.1M Na2-EDTA volumetric standard

• 0.1M Copper diamin-EDTA solution (e.g.: Merck 1052170500)
• Buffer-solution pH 10 (54 g ammonium chloride dissolved in 200 ml DI-water mixed with 350 ml of
ammonia 25 % and made up to 1000 ml with DI-water.)
Please follow the general regulations for hazardous materials in the Safety Data
Sheets!
The analytical procedure is to be followed exactly.
Be sure to observe all local regulations concerning the permitted limits for
pollutants.
Equipment required:
• usual laboratory equipment

• Titroprocessor with Cu-ISE and Ag/AgCl refrence, e.g. Metrohm 904 Titrando with Metrohm Cu-ISE
(Order No. 6.0502.140) and LL ISE Reference electrode (Order No. 6.0507.100) with Electrolyte
solution c(KCL)=3 M (only if a titroprocessor is used for the determination)
The above listed equipment is only valid when this method was created. For purchase of new
analytical equipment the recommend equipment list has to be followed:
https://10.187.127.52/Communication/html/scientific_services_chemical_services_analytics.php
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Operating Parameters (for Titroprocessor only)
Modus: Dynamic Titration U
Titrationspeed: Optimal
Stop EP: 1
EP crit.: 20
Procedure:
Manual titration:
• 1.0 ml** of the sample is transferred into a suitable vessel and mixed with
• 80 ml deionized water,
• 10 ml 25 % ammonia solution and
• 2 spatula tips of indicator triturate.
• Titrate with 0.1M Na2-EDTA volumetric standard to a deep purple endpoint. At the end of the titration
the EDTA volumetric solution should be added carefully, because of a slight delay of color change.
Potentiometric indication
• 1.0 ml** of the sample is transferred into a suitable vessel. Add

• 10 ml of 0.1 M Copper(NH4)2-EDTA solution and
• 20 ml of buffer pH 10. Wait 5 minutes and add
• 70 ml DI-water before titrating with 0.1M Na2-EDTA volumetric standard to the first endpoint.
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Evaluation:
The consumption of 0.1M Na2-EDTA volumetric standard in ml***, multiplied by 5.871 gives the content of
Nickel in g/l.
Example:
The titration of 1.0 ml sample consumed 8.50 ml 0.1M Na2-EDTA volumetric standard.
8.5 x 5.871 = 49.9 g/l Nickel
Quality assurance: For maintenance, calibration of measuring devices and the use of
standards and reference materials please refer to the corresponding guidelines.
* Unless otherwise stated, these are always analytical grade substances.

** Volumes given exact to a decimal point must be measured with a volumetric pipette.
*** For the purpose of calculation, the factor of the standard solution is assumed to be 1.000 and is
therefore not taken into account in the examples.
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Version: 06
Determination of Chloride by Titration Doc.-No.: A0000480-06
Reagents required*:
• Potassium chromate indicator solution (saturated)

• Silver nitrate volumetric solution 0.1 M
pollutants, including the general regulations for hazardous materials!
Procedure:
• 2.0 ml of the nickel bath are mixed in a 300 ml Erlenmeyer flask with
• 100 ml of DI water and, after the addition of a few drops of saturated potassium chromate indicator
solution, titrated with
• 0.1 M silver nitrate volumetric solution. The titration process is complete when the initially white
precipitate turns brownish.
Alternative: The Titration can be conducted as a turning point titration using a

titroprocessor equipped with an Ag/AgCl electrode to determine the endpoint.
The consumption of 0.1 M silver nitrate volumetric solution*** in ml – multiplied by 1.77 – gives the total
chloride content of the bath in g/l.
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Example:
7.6 ml of 0.1 M silver nitrate volumetric solution were used for the titration of 2.0 ml nickel bath.
Calculation:
7.6 x 1.77 = 13.5 g/l Chloride

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Version: 04
Determination of the Boric Acid Content by Titration
Doc.-No.: EXT-0352-TIT-04
Principle:
Acid-Base Titration
Reagents required*:
• Sodium Hydroxide volumetric solution 0.1 M

• Indicator solution (0.04 % solution of bromocresol purple in alcohol)
• Karion F liquid 1 l = 1.29 kg (manufacturer: E. Merck AG, Darmstadt) or mannitol (solid)
Procedure:
• 2.0 ml** sample solution are pipetted into a 300 ml Erlenmeyer flask and mixed with
• 10 ml of DI water and
• 1 ml of indicator solution.
The resulting solution is then neutralized drop by drop with
• 0.1 M sodium hydroxide volumetric solution until the solution turns purple. (Neutralization is not
necessary if the solution turns purple after the addition of the indicator solution.)
• 50 ml of Karion F liquid or equivalent 5 g of mannitol are then added to it and mixed up well, which
turns the solution golden yellow. Titration is now performed with
• 0.1 N sodium hydroxide volumetric solution until the color changes to purple.
Alternative: The Titration can be conducted as a turning point titration using a

titroprocessor equipped with a pH electrode to determine the endpoint.
Multiplying the number of ml 0.1 N sodium hydroxide volumetric solution*** used by 3.092 produces the
content of boric acid in the solution in g/l.
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Example:
For the titration of 2.0 ml of the sample solution 11.0 ml of 0.1 M sodium hydroxide volumetric solution was
used.
Calculation:
11.0 × 3.092 = 34.0 g/l boric acid

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Version: 02
Titrimetric Determination of Boric Acid
with Glycerin Citrate Solution ("Mixed Solution") Doc.-No.: EXT-0478-TIT-02
Reagents required*:
• "Mixed solution": 60 g of sodium citrate are dissolved in distilled water, and then add 600 ml glycerin to
it. Dissolve 2 g phenolphthalein in the minimum amount of warm alcohol (denaturated with benzol) and
add this to the citrate-glycerin solution. Make-Up to 1 l with distilled water. (If the mixture turns red after
the addition of phenolphthalein - as a result of alkali in the glycerin - it can be neutralized by means of
careful addition of 0.1 N sulphuric acid until the red discoloration just disappears.)
• Sodium Hydroxide volumetric solution 0.1 N
Procedure:
•
**
1.0 ml nickel bath are mixed in a 300 ml Erlenmeyer flask with
• 100 ml distilled water and
• 25 ml "mixed solution". This is then titrated with
• 0.1 N sodium hydroxide volumetric solution until the pale green colour of the solution changes to a
definite red or violet. Since the solution is viscous, it must be well stirred continuously as otherwise the
red colour forms on every drop of caustic soda solution added and only disappears when the solution is
well stirred.
Multiplying the number of ml 0.1 N caustic soda volumetric solution used by 6.184*** produces the boric acid
content of the bath in g/l.
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Example:
6.2 ml of 0.1 N sodium hydroxide volumetric solution were used for the titration of 1 ml nickel bath.
Calculation:
6.2 x 6.184 = 38.3 g/l boric acid

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Version: 03
Semilux 101 Make Up and Semilux 102 Brightener by LC
Doc.-No.: A0002273-03
Principle:
Reversed Phase High Efficiency Liquid Chromatography (HPLC) using UV-detection and external standards
Reagents required*:
Semilux 101 Make Up, reference material

Semilux 102 Brightener, reference material
Phosphoric acid 85 %, HPLC quality
Acetonitrile HPLC-MS quality
De-ionized water (Millipore quality)
Please follow the general regulations for hazardous materials in the Safety data
sheets!
pollutants.
Equipment required:
HPLC-System with diode array detector (DAD, recommended) or variable wavelength detector (VWD)
including a manual or automatic sampling device and a data processing or integration system
e.g. Waters Alliance 2695 with Waters 2996 or Waters 2487

Standard laboratory equipment
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Procedure:
Operating Parameter:
Operation Mode gradient

Eluent A 0.05 % H3PO4 in de-ionized water (Millipore quality)
(0.5 ml 85 % phosphoric acid in 1000 ml de-ionized water)
Eluent B Acetonitrile
Time Flow A [%] B [%]

0.01 1.0 100 0
3.00 1.0 100 0
8.00 1.0 0 100
8.01 1.0 100 0
11.00 1.0 100 0
Flow rate 1.0 ml/min

Analytical Column Atlantis T3 from Waters, 100 x 4.6 mm, 3 µm
Runtime 11 min
Injection volume 25 µl,
Ext. temperature 23 °C
Detection UV/VIS at λ = 229 nm Semilux 101 Make Up
λ = 269 nm Semilux 102 Brightener
Pressure approx.1400 psi
Evaluation Waters Millenium 32 V 3.05.01
The aforesaid listed equipment is only valid when this method has been created.
For purchase of new analytical equipment the recommend equipment list has to be followed:
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Standard solutions:
Semilux 101 Make Up stock solution 10 ml/l:
Exactly 1.0**ml of Semilux 101 Make Up is pipetted into a 100 ml volumetric flask and filled up with de-
ionized water.
Semilux 102 Brightener stock solution 10 ml/l:
Exactly 1.0 ml of Semilux 102 Brightener is pipetted into a 100 ml volumetric flask and filled up with de-
ionized water.
Standard Solutions:
Standard solutions with the following concentrations in water are prepared out of the stock solutions:
Mix A Mix B Mix C
Make Up 0.05 ml/l 0.1 ml/l 0.2 ml/l
Brightener 0.02 ml/l 0.04 ml/l 0.1 ml/l
The correct values have to be calculated out of the real concentrations in the certified references.
Sample Preparation
Depending on the contents the sample is diluted with de-ionized water in a way that the measured peak
areas are within the calibration curve.
Dilution example for the determination of:
Semilux 101 Make Up: 1:50, 1:20
Semilux 102 Brightener: 1:20, 1:10;
Evaluation:
Retention time: Semilux 102 Brightener approx. 1.6 min

Semilux 101 Make Up approx. 7.7 min
The contents of Semilux 101 Make Up and Semilux 102 Brightener are evaluated via linear external
calibration by using the instruments software.
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Example:
Fig.1: Example chromatogram of a sample solution 1:20 λ = 229 nm

0,40
7,664
0,30
AU
0,20
0,10
0,00
1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00 10,00
Minutes
Fig.1: Example chromatogram of a sample solution λ = 260 nm

1,616
0,030
0,020
AU
6,076
0,010
0,000
1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00 10,00 11,00
Minutes

Page: 23 / 28
10.07.2018 GPT DECO

Version: 05
Semilux 100
Version: 01
Semilux SE1 using LC-UV
Doc.-No.: A0003103-01
Principle: RP-HPLC with UV-VIS detection and external calibration
Reagents required*:
• Semilux SE1, 1000 ml/l, reference material

• H3PO4, 85 %
• Methanol, HPLC grade
• DI-water, Millipore-quality
Please follow the general regulations for hazardous materials in the Safety data sheets!
Be sure to observe all local regulations concerning the permitted limits for pollutants.
Equipment Parameter and Operating Parameter
HPLC-System
Model: Alliance or equivalent model
Mobile phase A: DI-water + 0.05 % H3PO4

Mobile phase B: Methanol
Flow rate: 1.3 ml/min

Pressure: 3000 PSI
Time in min A% B%
0 100 0
16 100 0
16.1 0 100
22.0 0 100
22.1 100 0
45 100 0
Page: 24 / 28
10.07.2018 GPT DECO

Version: 05
Semilux 100
Injection System
Model WATER Alliance or equivalent model

Injection volume 25 µl
Running time 45 min.
Column
Material LiChrospher 60 RP select B

Graining 5 µm
Length 250 mm
Diameter 4.6 mm
Detector
Detection UV/VIS at λ = 198 nm

Model WATERS 2487 or equivalent model
Sensibility 1.0
Int. temperature 25 °C
Ext. temperature 25 °C
Retention time
Semilux SE1: 10.4 min
The above listed equipment is only valid when this method was created. For purchase of new
analytical equipment the recommend equipment list has to be followed:
Page: 25 / 28
10.07.2018 GPT DECO

Version: 05
Semilux 100
Procedure
Stock Solution:
Exactly 1.0 ml Semilux SE1) is placed into a 100 ml measuring flask and the flask is filled up to the
mark with DI-water. (= 10 ml/l)
Standards for Calibration:
For external calibration the standards are prepared through corresponding dilutions of the stock solutions.
Water is used for the dilution.
concentration of Semilux SE1: 0.2 ml/l, 0.5 ml/l and 1.0 ml/l
Sample Preparation
The sample is measured undiluted and diluted in a ratio of 1:1. To 1 ml of the sample 1 ml DI-Water is added
and shaken.
The measured peak area of the sample must be between the peak areas of the standards. After
measurement the LC-system is to be cleaned for 15 min using Methanol/Water (1:1).
Calculation
The concentration of Semilux SE1 is calculated by external calibration through a suitable HPLC
software.
Page: 26 / 28
10.07.2018 GPT DECO

Version: 05
Semilux 100
Document of Analyses:
Image 1: sample chromatogram, undiluted sample

This sheet shall serve for your information. The content of the sheet is based on our best Atotech Deutschland GmbH
knowledge. We do not undertake any duty to advise. The contents of the sheet shall not P.O. Box: 21 07 80
be considered as an agreement on condition and quality of the goods delivered. 10507 Berlin, Germany
The decision to use our products for its production purposes is the responsibility of our Erasmusstraße 20
customer. We can accept liability only for the quality of our products at delivery. If 10553 Berlin, Germany
difficulties arise in the application of our products, we propose that you contact our phone +49 (0) 30 349 85 0
technical service department. fax +49 (0) 30 349 85 777
Page: 27 / 28
10.07.2018 GPT DECO

Version: 05
Semilux 100
9. Document History
Current revision status Date Change against last version:

01 21.June.2016 New
03 24.Mar.2017 No longer EXPT -> AI update
A0002273-02
04 07.Dec.2017 Changes from Mr Ewald and Mr Wachter
included; AI Update A0002273-03
05 07.June.2018 AI added A0003103-01
Page: 28 / 28
10.07.2018 GPT DECO

Semilux 100 Ds v05

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Semilux 100 Ds v05

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NICKEL Version: 05

Semilux 100 IMDS-No.: 114806927

Released on: Released by:

10.07.2018 GPT DECO

The Semilux 100 process is characterized by:

Tanks Mild steel with hard rubber lining, PVC as well as

Heating Heat exchanger, heating coils or immersion heaters made of

Anodes Rolled pure nickel anodes, electrolytic nickel anodes in

Anode Bags Required, use of twin bags is recommended.

Filtration Continuous. Pumps and filters (recommended: plate filter)

Applicable Filter Aid Diatomaceous earth or cellulose with activated carbon.

Released on: Released by:

10.07.2018 GPT DECO

stroke length double strokes/min

Released on: Released by:

10.07.2018 GPT DECO

Make-Up of 100 l Liter kg

Semilux 101 Make Up

Released on: Released by:

10.07.2018 GPT DECO

pH 4.0 (3.8 – 4.4)

Temperature 55 °C (52 – 62 °C)

Agitation Mechanical and / or air.

Cathode Current Density 4 A/dm² (2 – 5 A/dm²)

Anodic Current Density < 3 A/dm² in highly agitated tanks

Ratio Anode : Cathode 1.5 : 1 – 2 : 1

Rectifier DC with a ripple of < 5 %

Rate of Deposition 0.8 µm/minute at 4 A/dm²

Cathodic Current Efficiency 94 – 95 %

Released on: Released by:

10.07.2018 GPT DECO

Nominal values On make up During operation

Salt Nickel Chloride ions Boric Acid

Released on: Released by:

10.07.2018 GPT DECO

Function of the Additives

Consumption for 10,000 Ah

Semilux 101 Make Up

Semilux 102 Brightener

Semilux 102 Brightener consumption for 10,000 Ah at varying make up concentrations

Released on: Released by:

10.07.2018 GPT DECO

Semilux 103 Booster

Released on: Released by:

10.07.2018 GPT DECO

6. SAP No. for Make-Up and Maintenance Products

PRODUCT SAP No.

Released on: Released by:

10.07.2018 GPT DECO

7. Recommendations for Wastewater Treatment

Released on: Released by:

10.07.2018 GPT DECO

Principle: Complexometric titration

Reagents for manual titration:

• 0.1M Na2-EDTA volumetric standard

Reagents for titroprocessor:

• 0.1M Na2-EDTA volumetric standard

• usual laboratory equipment

Released on: Released by:

10.07.2018 GPT DECO

Operating Parameters (for Titroprocessor only)

Modus: Dynamic Titration U

• 1.0 ml** of the sample is transferred into a suitable vessel. Add