Argalux 64 Ds v11

Version: 11
PMP AG
Doc.-No.: 3074
DATA SHEET
SAP-No.: 1678676
Argalux 64
IMDS-No.: 757767
Hard Bright Silver Plating Process
CONTENTS
1.
Process Information............................................................................................................................... 2
2.
Equipment............................................................................................................................................. 2
3.
Make-Up with Potassium cyanide.......................................................................................................... 2
4.
Make-Up with Sodium cyanide.............................................................................................................. 3
5.
Working Parameters.............................................................................................................................. 4
6.
Process Control..................................................................................................................................... 4
Replenishment................................................................................................................................................. 4
Argalux 64 Hardener........................................................................................................................ 4
7.
Pre-treatment recommendations........................................................................................................... 6
8.
Silver Strike........................................................................................................................................... 6
Equipment........................................................................................................................................ 6
Make-Up with Sodium Cyanide........................................................................................................ 7
Make-Up with Potassium Cyanide.................................................................................................... 7
Maintenance..................................................................................................................................... 7
9.
Post-Treatment...................................................................................................................................... 8
10. SAP No. for Make - Up and Maintenance Products...............................................................................8
11.
General Safety Precautions................................................................................................................... 8
12. Recommendations for Wastewater Treatment.......................................................................................9
13. Analytical Instructions.......................................................................................................................... 10
Determination of Carbonate by Titration of the Precipitated Barium Carbonate.............................10
Determination of Carbonate by Direct Titration...............................................................................12
Determination of the Content of Free Cyanide by Titration.............................................................14
Silver in cyanidic silver baths by F-AAS.......................................................................................... 16
Determination of Silver with Ammonium Thiocyanate by Titration..................................................19
Argalux 64 Hardener by Photometry..............................................................................................21
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1. Process Information
Argalux 64 silver process has been designed to provide bright deposits with hardness values of
185 HV 0.15 +/-10 % over a wide CD operating range.
These deposit properties are well suited for cutlery and hollow-ware applications.
2. Equipment
Tanks
PVC, Polyethylene, Polypropylene as well as PVC /

Polyester composite material
Extraction
Required
Cathode agitation
Ideally 2.5 meters/ min using a stroke length of 100 mm at a

rate of 25/min
Anodes
Pure silver, 99.9% minimum

The anode area should be as large as possible. Inert anodes
should not be used.
Anode bags
Cotton cloth, fully synthetic special cloth
Filtration
Required; 1 volume turn-over per hour
3. Make-Up with Potassium cyanide

Make up of 100 l
Liter
kg
Potassium Silver Cyanide (54% Ag)

5.5
Silver Trisalyt Base
4.0
5.0
* Silver Trisalyt Conductive Salt
--(1.0)
(optional)
Potassium cyanide (NaCN free)
--13.5
Argalux 64 Brightener
0.4
0.4
Argalux 64 Hardener
1.5
1.66
* To enhance the throwing power, up to 20 g/l Silver Trisalyt Conductive Salt may be added.
Always use deionised water for the preparation of silver electrolytes and for correction of any
evaporation losses. The use of city 'mains' water may lead to reduced brightness or nonuniform brightness.
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Pre-dissolve the potassium silver cyanide (54%) and Silver-Trisalyt Base in approx 70% final volume of
deionised water, then add the potassium cyanide (sodium-free) and mix well until dissolved.
Then, either batch treat using approx 50 g of powdered activated carbon per 100lt electrolyte volume (ideally
low sulfur, low iron) and filter the bath thoroughly.
Alternatively, filter continuously for several hours over a pre-packed carbon filter, then replace the filter
cartridge.
Add the Argalux 64 Hardener, followed by Argalux 64 Brightener and continue to filter. Dilute to final
volume with deionised water and mix well.
4. Make-Up with Sodium cyanide

Make up of 100 l
Potassium Silver Cyanide (54% Ag)
* Silver Trisalyt Conductive Salt
(optional)
Sodium cyanide (96/98% NaCN)
Argalux 64 Hardener
Liter
kg
4.0
---
5.5
5.0
(1.0)
--0.4
1.5
10
0.4
1.66
Separately, overnight pre-purify the required sodium cyanide solution (using approx 15 % final volume of
water) see Process control section for details.
Pre-dissolve the potassium silver cyanide (54%) and Silver-Trisalyt Base in approx 70% final volume of
deionised water, then add the cleaned sodium cyanide solution (refer purification procedure in chapter
Process Control) and mix well until dissolved.
Then, either batch treat using approx 50 g of powdered activated carbon per 100lt electrolyte volume (ideally
low sulfur, low iron) and filter the bath thoroughly.
Alternatively, filter continuously for several hours over a pre-packed carbon filter, then replace the filter
cartridge.
Add the Argalux 64 Hardener, followed by Argalux 64 Brightener and continue to filter. Dilute to final
volume with deionised water and mix well.
IMPORTANT NOTE: In all work with Argalux 64, make sure that all regulations on
operations with cyanides are carefully observed.
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5. Working Parameters
Metal content
Approx. 30 g/l Ag
Density
Typically 1.12 g/cm at 20 C (15 B)
Temperature
15 25 C Higher temperatures will restrict the effective

plating range.
Voltage
Rack: approx.1 V; increasing to 4 V if larger anode to

cathode distances are used.
Barrel: typically 4 10 V
Current density
0.5 1.2 A/dm for rack operation

0.2 0.4 A/dm for barrel operation
Plating rate
Rack: 0.62 m/ minute at a current density of 1A/ dm.

Barrel: 0.12 m/ minute at 0.2 A/dm.
6. Process Control
Replenishment
For every 10,000 Ah (equivalent to 40 kg of silver) add the following:
Argalux 64 Hardener
Liter
kg
15 18
4.0
16.6 19.8
4.0
Ideally these additions should be made (with sufficient agitation) at the end of daily production and/ or after
10 % of Argalux 64 Brightener has been consumed..
Effect of constituents
Note: Please refer to Argalux 64 Supervision for Hull cell control and the effect of electrolyte constituents.
Argalux 64 Hardener
After lengthy idle periods, the Argalux Hardener activity may fall. This can be easily verified by Hull cell or
analysis and corrective action made prior to use.
This product has a limited shelf life and requires careful handling.
It must not be diluted if it is intended for auto-dosing. Ideally it should not be stored in part containers (best to
transfer a smaller bottle with minimum air gap). Any stored product exhibiting precipitations should be
replaced.
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Free Cyanide ion

In normal use, using an adequate surface area of soluble silver anode, the concentration of both the silver
and free cyanide ion should remain constant.
However in cases of high drag-out or insufficient anode area, small corrective additions may be required,
based on analysis.
Sodium Cyanide
Low free cyanide values should be corrected using 96 98%w/w sodium cyanide, which has
been purified overnight prior to addition.
The purification procedure is as follows:
For every 1 kg addition of sodium cyanide required, separately pre-dissolve in approx 2 litres of
DI water and slowly add with mixing approx 0.4 l of dilute (3 % (w/w)) hydrogen peroxide. Allow
to react overnight prior to adding to the Argalux 64 electrolyte.'
Note: This oxidation purification procedure will remove a small 'negligible' quantity of NaCN.
Ideally, the g/l sodium cyanide concentration should be 4 to 6 times the g/l silver level.
Potassium Cyanide
For situations where cyanide is used in preference to sodium, to raise the free cyanide content, high purity
grade potassium cyanide (sodium-free) should be used (note: large additions will result in solution cooling
due to the endothermic dissolution of potassium cyanide).
In the extreme situation where a large addition of potassium cyanide is required, the potassium cyanide
should be separately dissolved in a portion of the electrolyte, allowed to stand for a few hours and then
filtered prior to returning to the original solution.
In extreme cases where the free cyanide concentration exceeds the maximum limit (usually when inert
anodes are used), an addition of silver cyanide (80.5% w/w Ag), followed by dilution, should help to reduce
the concentration.
Silver
To raise the silver metal concentration by 1 g/l, add 1.85 g/l potassium silver cyanide (54% Ag) and 2.0 g/l
Silver Trisalyt Replenisher.
Because of the silver content raise slowly, a metal analyse should made in longer periods (every 1 to 2
month).
Carbonate concentration.
Silver Cyanide electrolytes are strongly alkaline and as a result of atmospheric carbon dioxide and electrolyte
breakdown, Potassium Carbonate will be formed. High levels of this by-product will cause a lack of throwing
power and cause a reduction in the effective plating range due to high CD burning.
Sodium carbonate has reduced solubility (compared to silver cyanide complexes) and it may be possible to
freeze out by simply cooling the electrolyte.
Potassium Carbonate, however has a very high solubility and hence is only practically removed by
precipitation. At levels > 100 g/l, it is recommended that the electrolyte is batch treated with the product
Decarbonate AG using the following procedure:
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1. Transfer electrolyte into a treatment tank, preferably fitted with a mechanical stirrer.
2. Heat the solution to approx. 30 C and slowly add the required quantity of Decarbonate AG to the region
of strongest agitation.
3. Mix the electrolyte for 1 hour, then switch off the mixer and allow solution to settle, preferably overnight.
4. Filter the solution back into the production tank, preferably though a finer filter cartridge.
5. The electrolyte is now ready to use.
Calculation:
1 kg of Decarbonate AG will treat 0.78 kg of Potassium Carbonate
For every 100 g/l of Potassium Carbonate to be removed, add 128 g/l Decarbonate AG.
Note: It is only recommended for a maximum of 2x treatments, otherwise a reduced CD range may be
observed.
7. Pre-treatment recommendations
Copper and alloy components require simple cleaning and activation prior to silver plating. However,
substrate containing lead, tin, zinc or iron must be pre-plated with cyanide copper prior to applying a silver
deposit.
8. Silver Strike
Equipment
Tanks
Mild steel lined with suitable hard rubber or PVC, tanks of

self-supporting PVC or polyethylene
Anodes
Stainless steel (18 Cr Ni 8)
Solution voltage
Rack plating: 3 - 4 V
Barrel plating: 3 - 8 V
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Make-Up with Sodium Cyanide

Make-up of 100 l
Di water
Potassium solver cyanide (54% Ag)
Sodium cyanide (overnight purified)
Liter
kg
approx. 90
approx. 90
0.28
0.25
7.5
0,2
Distilled water should be used for making up silver baths.
Make-Up with Potassium Cyanide

Make-up of 100 l
Di water
Potassium solver cyanide (54% Ag)
Potassium cyanide (sodium free)
Liter
kg
approx. 90
approx. 90
0.28
0.25
10.0
0,2
Silver Strike duration

3 - 30 seconds using slow cathode movement. Rack components are generally silver-struck for a maximum
of 10 seconds, whereas a maximum of 30 seconds may be required for open-ended and submerged plating
barrels in automatic plants.
The silver-struck components can be transferred directly to the Argalux 64 electrolyte without the need for
rinsing.
Maintenance
The silver consumed in the silver strike solution may be replenished as required. Ideally, the silver content of
the silver strike solution should be 1 - 3 g/l. If the silver concentration falls below 1 g/l or if it exceeds 3 g/l
there may be a risk of adhesion failure, observed as surface blisters.
To raise the silver metal concentration by 1 g/l, add 1.85 g/l potassium silver cyanide (54% Ag) and 2.0 g/l
Silver Trisalyt Replenisher.
The performance of the silver strike can be monitored periodically by immersing by dipping a thoroughly
cleaned copper panel into the silver strike solution without applying power. No immersion silver coating
should be observed within the first 15 seconds. If this test fails, then small additions of potassium or sodium
cyanide should be added until a pass is observed.
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9. Post-Treatment
To prevent staining or 'spotting' after plating (particularly for substrates containing pores or other defects), it
is advisable, after initial rinsing, to immerse into a 3% v/v dilute acetic acid solution, followed by further
rinsing stages. This will help to effectively neutralise any electrolyte traces and prevent any staining or
'spotting'
10. SAP No. for Make - Up and Maintenance Products

PRODUCT
SAP No.
SILVER TRISALYT BASE

SILVER TRISALYT REPLENISHER
SILVER TRISALYT CONDUCTIVE SALT
ARGALUX 64 BRIGHTENER
ARGALUX 64 HARDENER
DECARBONATE AG
1687428
1685787
1685788
396010
396408
1684950
11. General Safety Precautions

Avoid direct contact with this material. Do not inhale associated mist or vapors. Wash contaminated clothing
before reuse. Refer to Material Safety Data Sheet (MSDS) for specific precautions before handling this
material and for first aid recommendations. As applicable, keep exposure below the limits recommended by
the appropriate regional regulatory agencies.
For further information on product safety refer to the corresponding MSDS. The
MSDS is enclosed at the first delivery of a product. Otherwise a MSDS for a product
is available on request from the appropriate regional Atotech office.
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12. Recommendations for Wastewater Treatment

Rinse waters and concentrates of Argalux 64 must always be subjected to special treatment due to the
containing cyanide and possible complexing agents.
Rinse Water
The rinsing steps after silver plating should be designed in such a manner that the dragged-out silver can be
effectively recovered by suitable recycling techniques. A strong alkaline ion exchanger (e.g. Lewatit
MonoPlus M 500) can be used for this purpose at a concentration of maximum 2 mval Ag/l.
Once all the silver has been removed from the rinsewater, it may be directly sent to the final neutralization
process. The ion-exchanger resin which has become loaded with silver can be sent to a special company for
recovery of the silver.
If there is cyanide which is easily releasable, a cyanide oxydation has to be carried out supplementary.
If no recovery system exists on the drag-out rinse after using Argalux 64, the containing cyanide has to be
treated first by an oxydation followed by a heavy metal precipitation .The heavy metals can be precipitated
either by a neutralization precipitation at pH 10-11 or using sodium sulfide at pH 6-8..
Add sodium sulphide solution (10 15 %) until a significant potential jump can be recognized during a
potentiometric measurement or until lead acetate paper shows a brown color. After a reaction time of 10 min
remove the weak sulphide excess with a small amount of iron-III-chloride solution (about 10 %). The lead
acetate paper should no longer be brown in color.
Then adjust the pH to 9 with caustic soda / calcium hydroxide.
For better flocculation add flocculation agent (we recommend polyacryl amide/anionic with a mol mass of 4
6 million) and stir. Allow the precipitate to settle for better filtration over a special filter press.
After filtration is complete the filtrate must not be mixed with metal ions bearing waste streams.The filtrate
must be sent to the final neutralization process, bypassing the waste water treatment plant.
Concentrates
When silver is to be recycled, it is generally necessary to treat these silver solutions
separately from other solutions.
The following recycling methods are typical, although others can be recommended:
Electrowinning of silver using an appropriated electrolytic cell, followed by an oxydation
of the remaining cyanide.
Treatment of silver concentrate, or of a precipitated silver sludge, by a specialized recycling company.
If these methods cannot be used, the silver concentrate must be diluted in a ratio of 1 : 10 before sending to
the wastewater treatment plant. This treatment is carried out as described above.
Be sure to observe all local regulations concerning the limit values of pollutants
including the general regulations on dangerous materials!!
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13. Analytical Instructions

Determination of Carbonate by Titration of the Precipitated
Barium Carbonate
Version: 01
Doc.-No.: EXT-0344-TIT-01
Reagents required*:
Ammonium chloride
Ammonia conc. (density 0.91)
Barium chloride solution 1 M (244 g/l BaCl2 2 H2O)
Methylorange indicator solution 0.1 %

Hydrochloric acid volumetric solution 0.5 N
Be sure to observe all local regulations concerning the permitted limits for
pollutants, including the general regulations for hazardous materials!
Procedure:
10.0 ml** bath are allowed to run into a 250 ml glass beaker,
2 g solid ammonium chloride,
2 ml ammoniac conc. and
100 ml distilled water added to it and the solution heated almost to boiling point.
20 ml 1 m barium chloride solution are then added to it while stirring well. After the precipitate has
settled, the solution is filtered while still hot and the precipitate washed out well with hot distilled water
(about three to five times) until the flowing filtrate no longer turns red litmus paper blue. The washed-out
filter with precipitate on it is then returned to the precipitation beaker and about 100 ml hot distilled
water and
2 - 3 drops methylorange indicator solution added to it. Titration is then performed against
0.5 N hydrochloric acid volumetric solution until the yellow solution turns red and no longer turns yellow
again even after 1 - 2 minutes have passed.
The number of ml 0.5 n hydrochloric acid volumetric solution used***
multiplied by 2.65 produces the sodium carbonate content of the bath

multiplied by 3.45 produces the potassium carbonate content of the bath in g/l
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Example:
The following amount was used for the titration of 10.0 ml bath:
15.2 ml 0.5 n hydrochloric acid volumetric solution
Calculation:
15.2 x 2.65 = 40.3 g/l sodium carbonate
15.2 x 3.45 = 52.4 g/l potassium carbonate
*
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: 01
Determination of Carbonate by Direct Titration
Doc.-No.: EXT- 0345-TIT-01
Reagents required*:
Sodium chloride
Silver nitrate solution 1 N (170 g/l AgNO3)
Phenolphthalein indicator solution, 1 % in alcohol

Hydrochloric acid volumetric solution 0.5 N
Procedure:
10.0 ml** bath are diluted in a 300 ml Erlenmeyer flask with

100 ml distilled water. After the addition of
2 g solid sodium chloride, somewhat more than a fifth of
1 N silver nitrate solution of that amount of
0.1 N silver nitrate volumetric solution which was used for the cyanide titration with a
5.0 ml bath sample is added while shaking vigorously.
If, for example, 14.5 ml 0.1 N silver nitrate volumetric solution were used in a matt silver bath
(5.0 ml bath sample), then 14.5 : 5 = about 3 ml 1 N silver nitrate solution should be added.
If 24.2 ml 0.1 N silver nitrate volumetric solution were used in a bright- silver bath
(2.5 ml bath sample), then (24.2 x 2) : 5 = about 10 ml 1 N silver nitrate solution should be added.
After this, a few drops of phenolphthalein indicator solution are added and titration performed against 0.5 N
hydrochloric acid volumetric solution until the red solution becomes completely colorless.
The number ml 0.5 N hydrochloric acid volumetric solution used***
multiplied by 5.3 produces the sodium carbonate content of the bath

multiplied by 6.9 produces the potassium carbonate content of the bath in g/l.
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Example:
The following amount was used for the titration of 10.0 ml bath:
7.6 ml 0.5 N hydrochloric acid volumetric solution
Calculation:
Remarks
If a bath contains hydroxide (the pH value is then higher than 12.0), the hydroxide must be titrated in a
second sample, to which 20 ml of a 1 M barium chloride solution (244 g/l BaCl 2 H O) are added in
2
addition to the above-stated amounts of sodium chloride, 1 N silver nitrate solution and phenolphthalein
indicator solution. The ml 0.5 N hydrochloric acid volumetric solution used for this process are to be
subtracted from the first titration result.
Example
The following amount was used for titration without the addition of 1 M barium chloride solution:
The following amount was used for titration after the addition of 1 M barium chloride solution:
Calculation:
12.6 ml 0.5 N hydrochloric acid volumetric solution = amount used for carbonate +
hydroxide
- 5.0 ml 0.5 N hydrochloric acid volumetric solution = amount used for hydroxide
= 7.6 ml 0.5 N hydrochloric acid volumetric solution = amount used for carbonate
*
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Version: 02
Determination of the Content of Free Cyanide by Titration
Principle:
Redox titration
Required reagents*:
Ammonia solution 5 N (375 ml/l ammonia conc., density 0.91)

Potassium iodide solution 1 M (166 g/l potassium iodide)
Silver nitrate volumetric solution 0.1 N
Procedure:
5.0 ml** bath in the case of matt-silver baths

2.5 ml** bath in the case of bright-silver and flash-silver baths
(10.0 ml** bath are poured into a 100 ml graduated flask, which is then filled up to the mark with distilled
water. After mixing well 50.0 ml** = 5.0 ml or 25.0 ml** = 2.5 ml original bath are removed from the flask.)
The bath sample is diluted in a
300 ml Erlenmeyer flask with

100 ml DI water and mixed with
5 ml of 1 M Potassium iodide solution and
5 ml of 5 N Ammonia solution. Titration with
0.1 N Silver nitrate volumetric solution is then performed until the precipitate which forms on entry of the
drops no longer resolves after being shaken several times, but causes general turbidity of the solution.
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The volume in ml of the 0.1 M Silver nitrate standard solution*** used for the titration of 5 ml sample,
multiplied by 1.96, gives the content of free Sodium cyanide in g/l.

multiplied by 2.60, gives the content of free Potassium cyanide in g/l.
The volume in ml of the 0.1 M Silver nitrate standard solution*** used for the titration of 2.5 ml sample,
multiplied by 3.92, gives the content of free Sodium cyanide in g/l.

multiplied by 5.20, gives the content of free Potassium cyanide in g/l.
Examples
a) The following amount was used for the titration of 5.0 ml bath:
14.5 ml of 0.1 N Silver nitrate volumetric solution
Calculation:
14.5 x 1.96 = 28.4 g/l free Sodium cyanide
14.5 x 2.60 = 37.7 g/l free Potassium cyanide
b) The following amount was used for the titration of 2.5 ml bath:
24.2 ml of 0.1 N Silver nitrate volumetric solution
Calculation:
24.2 x 3.92 = 94.9 g/l free Sodium cyanide
24.2 x 5.20 = 125.8 g/l free Potassium cyanide
*
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Version: 01
Silver in cyanidic silver baths by F-AAS
Doc.-No.: A0002247-01
Principle:
The silver-containing sample is diffused and atomized in a compression air/acetylene-flame and the
absorption is measured at a wavelength of 328.1 nm. The determination is carried out through
external calibration by using corresponding standard solutions.
Reagents required:
Nitric Acid (HNO3), conc. (65 %), e.g. by Merck
Silver standard solution: 1000 mg/l
DI water
Please follow the general regulations for hazardous materials in the Material safety
data sheets!
The analytical procedure is to be followed exactly.
pollutants.
Equipment required:
Atomic Absorption Spectrometer with control and evaluation unit (e.g. Perkin Elmer, Varian)
Burner: Air/Acetylene one-slit burner head
Hollow cathode lamp: Silver
Operating mode
Absorption
Gas mixture
Compression air/acetylene
Lamp current
8 mA
Fuel flow
2.0 L/min
Integration time
1.0 s
Oxidant flow
13.5 L/min
Replicates
Wavelength
328.1 nm
Background correction
OFF
Slit
0.5 nm
Delay
30 sec
Calibration
New Rational
Rinse time
25 s
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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:
https://10.187.127.52/Communication/html/scientific_services_chemical_services_analytics.php
Procedure:
Calibration procedure:
0.5 mg/l Ag: 50 L of silver standard solution and 2 ml of nitric acid are pipetted into a 100 mlflask then
filled up to the mark with DI water and homogenized.
1 mg/l Ag:
100 L of silver standard solution and 2 ml nitric acid are pipetted into a 100 ml flask then filled
up to the mark with DI water and homogenized.
2 mg/l Ag:
200 L of silver standard solution and 2 ml of nitric acid are pipetted in to a 100 ml flask then
filled up to the mark with DI water and homogenized.
Sample preparation:
IMPORTANT NOTE:
The substance contains cyanide which on contact with acids will produce
hydrocyanic acid gas (HCN).
All operations have to be carried out under the fume cupboard!
1.0 ml** and 0.5 ml** of sample are pipetted into a 100 ml volumetric flask (dilution: 1:100/1:200)
Prior to analysis the sample hast to be further diluted (1:100):
1 ml** of each pre-diluted sample (1:100/1:200) is pipetted into a 100 ml volumetric flask.
Add 50 ml of deionized water and then (carefully!!!) add 4.0 ml of nitric acid.
After that the flask is filled up to the mark with deionized water.
the homogenized solution is analyzed at a wavelength of 328.1 nm
Evaluation:
The determination of the Ag content in the diluted sample is carried out automatically through the PCsoftware via the external calibration, which was carried out before. The determined silver concentration C Ag
[mg/l] for the diluted sample must be multiplied with the dilution factor. The determined silver content must be
within the calibration curve, otherwise another dilution has to be chosen.
CAg [mg/l] dilution factor = mg/l of Ag in the sample.
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Example:
1.13 mg/l 10000 = 11.3 g/l of silver
Quality assurance: For maintenance, calibration of measuring devices

and the use of standards and reference materials please refer to the
corresponding guidelines.
*
**

Volumes given exact to a decimal point must be measured with a volumetric pipette.
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Determination of Silver with Ammonium Thiocyanate by

Titration
Version: 03
Reagents required*:
sulfuric acid conc. (density 1.84)

nitric acid conc. (density 1.40)
Iron(III)-ammonium sulphate solution 0.4 M (19.3 g NH 4Fe(SO4)2 x 12 H2O + 10 ml H2SO4 5M topped
up to 100 ml with distilled water)
Ammonium thiocyanate volumetric solution 0.1 M
data sheets!
pollutants.
Procedure:
2.5 ml** silver bath are transferred into a 250 ml Erlenmeyer flask. After the addition of
10 ml distilled water,
3 ml of the sulphuric acid and 4.5 ml nitric acid added carefully.
IMPORTANT NOTE:
The substance contains cyanide which on contact with acids will produce hydrocyanic acid
gas (HCN) All operations have to be carried out under the fume cupboard!
Heat the flasks until all the deposit have disappeared and the solution has boiled for
5 - 10 minutes. After cooling down it is diluted with
90 ml distilled water. After the addition of
1.0 ml 0.4 M iron(III)-ammonium sulphate solution. Titration is performed against
0.1 M Ammonium thiocyanate volumetric solution until the whitish turbid solution turns bright-red/brown.
Alternative: The Titration can be conducted as a turning point titration

using a titroprocessor equipped with a platinium electrode to
determine the first endpoint.
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Version: 11
Argalux 64
Doc.-No.: 3074
Evaluation:
The number of ml 0.1 M Ammonium thiocyanate volumetric solution used *** multiplied by 4.315 produces the
silver content of the bath in g/l.
Example:
The following amount was used for the titration of 2.5 ml silver bath:
7.84 ml 0.1 N ammonium thiocyanate volumetric solution***
7.84 x 4.315 = 33.8 g/l silver


given exact to a decimal point must be measured with a volumetric pipette.
***
For the purpose of calculation, the factor of the standard solutions is assumed to be
1.000 and is therefore not taken into account in the examples.
** Volumes
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Version: 11
Argalux 64
Doc.-No.: 3074
Version: 03
Argalux 64 Hardener by Photometry
Doc.-No.: A0000870-03
Principle:
The Hardener produces a violet color complex in the Toluene phase with Rhodamine B, which can
be used for the photometrical determination.
IMPORTANT NOTE:
The sample contains cyanide which on contact with acids will produce hydrocyanic acid
gas (HCN).
All operations have to be carried out under the fume cupboard!
Reagents required*:
Antimony (III) standard solution (1 g/l), e.g. Merck 1.70302.0100

Hydrochloric acid 5 M
Sulfuric acid 2.5 M
Rodamine B solution (0.3 % in water)
Ammoniumetavanadate solution 0.01M (117 mg NH 4VO3 dissolved in 100 ml 1M HCl)
Toluene p.a.
DI-water
data sheets!
pollutants.
IMPORTANT NOTE:
Toluene is explosive and evaporate at room temperature.
All operations with Toluene have to be carried out under the fume cupboard!
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Version: 11
Argalux 64
Doc.-No.: 3074
Equipment required:
50 ml beakers
100 ml volumetric flasks
Separation funnel
variable pipettes
UV/VIS spectrometer (e.g. Lambda 2S Perkin Elmer)
Glass- or single-use plastic cuvettes (pathlength 1 cm)
Operating Parameter UV/VIS Spectrometer:

Method
Wavelength
565 nm
Curve
linear
ordmode
single wave
Procedure:
Standard preparation:
0.25 ml** of the Antimony standard solution is pipetted into a 100 ml volumetric flask. After addition of 20 ml
2.5 M Sulfuric acid the flask is filled up with DI-water (c Sb = 2.5 mg/l).
Sample preparation:
In a 50 ml beaker 10 ml 2.5 M Sulfuric acid is added to 1 ml bath (Vx) and while stirring filtrated into a 100 ml
volumetric flask. The precipitation on the filter is washed with 20 ml DI-water. To this solution subsequently
10 ml 2.5 M Sulfuric acid is added. The flask is filled up to 100 ml with DI-water.
Then process standard and diluted sample as follows below:
2 ml of the solution is placed into a 50 ml separation funnel

5 ml 5 M Hydrochloric acid,
2 ml of a 0.3 % Rhodamine B solution,
1 ml of a 0.01 M NH4VO3 solution is added.
Immediately 5 ml Toluene are added, the flask is closed with a plug and shaken for 1 min.
During shaking the flask has to be vented from time to time to avoid a pressure overload.
After separating the Toluene phase, colorized due to the presence of Hardener, is transfarred completely into
a clean vessel.
Immediately 5 ml Toluene are added again to the sample solution, the flask is closed with a plug and
shaken for 1 min.
During shaking the flask has to be vented from time to time to avoid a pressure overload.
After separating the Toluene phase, colorized due to the presence of Hardener, is merged with the former
organic phase and measured at 565 nm in 1 cm cuvettes against Toluene as blank.
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Version: 11
Argalux 64
Doc.-No.: 3074
Evaluation:
E sample c standard
E standard
2.59 = c(ml/l) Argalux 64 Hardener
Example:
E(std) = 0.496
E(sample) = 0.746
c(std) = 2.5
0.746 2.5
0.496
2.59 = 9.7 ml/l Argalux 64 Hardener
LOQ = 1.0 ml/l Argalux 64 Hardener

*
**

Volumes given exact to a decimal point must be measured with a volumetric pipette.
This sheet shall serve for your information. The content of the sheet is based on our best
knowledge. We do not undertake any duty to advise. The contents of the sheet shall not
be considered as an agreement on condition and quality of the goods delivered.
The decision to use our products for its production purposes is the responsibility of our
customer. We can accept liability only for the quality of our products at delivery. If
difficulties arise in the application of our products, we propose that you contact our
technical service department.
Atotech Deutschland GmbH

P.O. Box: 21 07 80
10507 Berlin, Germany
Erasmusstrae 20
10553 Berlin, Germany
phone +49 (0) 30 349 85 0
fax +49 (0) 30 349 85 777
Page: 23 / 23
Released on:
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BTT PMP

Argalux 64 Ds v11

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Hard Bright Silver Plating Process

Hard Bright Silver Plating Process

PVC, Polyethylene, Polypropylene as well as PVC /

Ideally 2.5 meters/ min using a stroke length of 100 mm at a

Pure silver, 99.9% minimum

Cotton cloth, fully synthetic special cloth

Required; 1 volume turn-over per hour

3. Make-Up with Potassium cyanide

Potassium Silver Cyanide (54% Ag)

Hard Bright Silver Plating Process

4. Make-Up with Sodium cyanide

Hard Bright Silver Plating Process

Typically 1.12 g/cm at 20 C (15 B)

15 25 C Higher temperatures will restrict the effective

Rack: approx.1 V; increasing to 4 V if larger anode to

0.5 1.2 A/dm for rack operation

Rack: 0.62 m/ minute at a current density of 1A/ dm.

Hard Bright Silver Plating Process

Free Cyanide ion

Hard Bright Silver Plating Process

Mild steel lined with suitable hard rubber or PVC, tanks of

Stainless steel (18 Cr Ni 8)

Hard Bright Silver Plating Process

Make-Up with Sodium Cyanide

Distilled water should be used for making up silver baths.

Make-Up with Potassium Cyanide

Silver Strike duration

Hard Bright Silver Plating Process

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

SILVER TRISALYT BASE

11. General Safety Precautions

Hard Bright Silver Plating Process

12. Recommendations for Wastewater Treatment

Hard Bright Silver Plating Process

13. Analytical Instructions

Methylorange indicator solution 0.1 %

The number of ml 0.5 n hydrochloric acid volumetric solution used***

multiplied by 2.65 produces the sodium carbonate content of the bath

Hard Bright Silver Plating Process

Hard Bright Silver Plating Process

Determination of Carbonate by Direct Titration

Doc.-No.: EXT- 0345-TIT-01

Phenolphthalein indicator solution, 1 % in alcohol

10.0 ml** bath are diluted in a 300 ml Erlenmeyer flask with

multiplied by 5.3 produces the sodium carbonate content of the bath

Hard Bright Silver Plating Process

Hard Bright Silver Plating Process

Determination of the Content of Free Cyanide by Titration

Ammonia solution 5 N (375 ml/l ammonia conc., density 0.91)

5.0 ml** bath in the case of matt-silver baths

300 ml Erlenmeyer flask with

Hard Bright Silver Plating Process

multiplied by 1.96, gives the content of free Sodium cyanide in g/l.

multiplied by 3.92, gives the content of free Sodium cyanide in g/l.

Hard Bright Silver Plating Process

Silver in cyanidic silver baths by F-AAS

Hard Bright Silver Plating Process

Hard Bright Silver Plating Process

Quality assurance: For maintenance, calibration of measuring devices

Unless otherwise stated, these are always analytical grade substances.

Hard Bright Silver Plating Process

Determination of Silver with Ammonium Thiocyanate by