Professional Documents
Culture Documents
PMP AG
Doc.-No.: 3152
DATA SHEET
SAP-No.: 1679919
Silverlume PLUS
IMDS-No.: 757767
CONTENTS
1.
2.
3.
4.
5.
6.
7.
8.
11.
12.
13.
14.
15.
16.
Process Information............................................................................................................................... 2
Equipment............................................................................................................................................. 2
Working Parameters.............................................................................................................................. 3
Make-Up................................................................................................................................................ 3
Make-Up Sequence............................................................................................................................... 4
Operating Conditions............................................................................................................................. 5
Maintenance.......................................................................................................................................... 5
Process Control..................................................................................................................................... 6
Pre-treatment Recommendations.......................................................................................................... 8
Equipment........................................................................................................................................ 8
Make-Up........................................................................................................................................... 8
Maintenance..................................................................................................................................... 9
Post-Treatment...................................................................................................................................... 9
SAP No. for Make - Up and Maintenance Products...............................................................................9
General Safety Precautions................................................................................................................... 9
Recommendations for Wastewater Treatment.....................................................................................10
Analytical Instructions.......................................................................................................................... 12
Silverlume B Plus by LC................................................................................................................. 12
Determination of Carbonate by Titration of the Precipitated Barium Carbonate.............................15
Determination of Carbonate by Direct Titration...............................................................................17
Determination of the Content of Free Cyanide by Titration.............................................................19
Silver in cyanidic silver baths by F-AAS.......................................................................................... 21
Determination of Silver with Ammonium Thiocyanate by Titration..................................................24
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1. Process Information
Silverlume PLUS is a bright silver plating process, which is extremely versatile and simple to control.
Silverlume PLUS provides brilliant white deposits from both rack and barrel applications and can be
used for all decorative and industrial requirements.
Silverlume PLUS provides uniform bright white deposits with typical hardness value of 80 HV 0.15 +/10 % and electrical resistivity value of approx 1.7/cm.
Silverlume PLUS is based on an organic based brightener system that may also provide some
corrosion protection benefits.
2. Equipment
Tanks
Agitation
Exhaust
Essential
Filtration
Bath temperature
15 - 25 C
Higher temperatures will restrict the effective plating range.
Anodes
Anode bags
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Heaters
Electrical Supply
3. Working Parameters
pH
14 ( 13 14)
Bath voltage
4. Make-Up
Make-Up of 100 lt
Rack Operation
Barrel Operation
5.5 kg
3.7 kg
10.0 kg
10.0 kg
5.0 kg (0.4 l)
5.0 kg (0.4 l)
(2.0 kg)
(2.0 kg)
Silverlume A PLUS
0.12 kg (0.12 l)
0.12 kg (0.12 l)
Silverlume B PLUS
0.325 kg (0.325 l)
0.325 kg (0.325 l)
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5. Make-Up Sequence
The following sequence refers to equipment which has been prepared, rinsed with DI-Water and drained.
1.) Add approximately half of the required amount of DI-Water to the tank/ sump.
2.) Switch on the extraction and carefully add the required quantity of Potassium Cyanide and EXPT
Silbertrisalyt Conductive Salt, and mix well.
3.) Carefully add the required quantity of Potassium Silver Cyanide (54% Ag) and EXPT Silbertrisalyt
Base, and mix well to completely dissolve.
Optional stages - recommended for improved quality work and trouble-free operation:
3.a)
Either circulate through a carbon pack filter cartridge or batch carbon treat overnight in a
separate tank (using 0.5 1.0 g/l of activated carbon powder).
3.b)
Remove carbon filter or filter the electrolyte from the treatment tank into the production unit,
replacing filter with normal pre-rinsed polypropylene filter. Confirm effective treatment by 0.2 A,
10 min Hull cell if possible (uniform matt panel confirms the absence of any organic
contamination).
4.)
Switch on filter pump and solution agitation system (if used) and circulate for at least 30 minutes.
Heating, if required, should be switched on at this stage.
5.)
Add the required quantities of Silverlume A PLUS and Silverlume B PLUS and mix very well,
preferably for several hours.
6.)
Remove a small sample (500 ml) for day-1 analysis (this will also serve later as a performance
standard).
7.)
When working with the high-performance Silverlume PLUS the regulations concerning the handling
of cyanide solutions must be observed.
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6. Operating Conditions
Optimum (Range)
Silver concentration (g/l)
(rack)
(barrel)
30 (20 40)
20 (10 30)
Temperature (C)
20 (18 25)
Higher temperature reduce throwing power of the
brightness.
(rack)
(barrel)
(rack)
(barrel)
67 mg/Amin (100 %)
1 micron in 1.6 min at 1 A/dm
1 micron in 5.33 min at 0.3 A/dm
Agitation
7. Maintenance
For every 10,000 Ah (equivalent to 40 kg of deposited silver) add the following:
kg
Silverlume A Plus
Silverlume B Plus
2.0 2.5
0.4 0.8
Ideally these additions should be made (with sufficient agitation) at the end of daily production and/ or after
10 % of Silverlume A PLUS has been consumed.
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8. Process Control
Potassium Cyanide
In normal use, using an adequate surface area of soluble silver anode, the concentration of both the Silver
and free Potassium Cyanide should remain constant.
However in cases of high drag-out or insufficient anode area, small corrective additions may be required,
based on analysis.
To raise the free Potassium Cyanide level, 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 cases where the free Potassium Cyanide level exceeds the maximum limit (usually when inert anodes are
used), an addition of Potassium 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 EXPT Silvertrisalyt Replenisher.
Potassium Carbonate
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. Potassium Carbonate 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.
Silverlume A PLUS
Silverlume A PLUS is the primary organic brightener and requires frequent maintenance. High levels of
Silverlume A PLUS can result in a grainy or streaked appearance. Correction can be made by carbon
purification.
Silverlume B PLUS
Silverlume B PLUS is the essential wetting agent required to maximise the effect of
Silverlume A PLUS over a wide plating range. Excess of Silverlume B PLUS can lead to low CD haziness
and restrict the high CD limit. Correction can be made by carbon purification.
1.66 / cm
80 HV
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PVC, or sheet steel with hard rubber lining, tanks of selfsupporting PVC or polyethylene
Anodes
Bath voltage
Make-Up
Make-up of 100 l
Liter
kg
0.2
0.28
0.25
10.0
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Maintenance
The silver concentration needs to be maintained within the range 1 - 3 g/l. when required by the addition of
Potassium Silver Cyanide (54% Ag). Adhesion concerns may occur if the silver concentration falls below 1 g/l
or exceeds 3 g/l.
The performance of the silver strike can be confirmed by simple immersion (without current) of a precleaned/ acid activated copper or brass test panel. A minimum duration of 15 s prior to immersion coating
indicates satisfactory condition of the silver strike. Less than 15 s indicates the need to increase the free
cyanide content until a pass is achieved.
12. Post-Treatment
Certain substrates (with pores or other inhomogenities), may cause surface spots or blooms to form (due to
entrapment of electrolyte residues) after silver-plating. To prevent this situation occurring, it is recommended
to immerse the rinsed articles in 3 %w/w acetic acid post dip with further thorough rinsing.
SAP No.
1687428
1685787
1685788
1683400
1682998
1684950
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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 oxidation 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 waste water 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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Silverlume B Plus by LC
Doc.-No.: A0002280-01
Principle:
Reversed Phase High Efficiency Liquid Chromatography (HPLC) using UV-detection and external standards
Reagents required:
Silverlume B Plus, 1000 ml/l 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 Material 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:
HPLC-system with manual or automatic sampling UV-detector, data processing- or
integration system
Standard laboratory equipment
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
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Procedure:
Operating Parameter:
Operation Mode isocratic
Eluent A
0.1 % H3PO4 in de-ionized water (Millipore quality)
(1.0 mL 85 % phosphoric acid in 1000 mL de-ionized water)
Eluent B
Acetonitrile
Time
0.0
3.0
Flow
1.5
1.5
A [%]
80
80
B [%]
20
20
Flowrate
1.5 mL/min
Analytical Column
Purospher Star RP-18 endcapped from Merck, 55 x 4 mm, 3 m
Runtime
3 min
Injection volume 5 L,
Ext. temperature:
25 C
Detection
UV/VIS at = 254 nm
Pressure
approx. 1500 - 2000 psi
Evaluation
Waters Millenium 32 V 3.05.01
Standard solutions:
Silverlume B Plus stock solution:
Pipette 0.5 mL** of Silverlume B Plus in a 100 mL volumetric flask and fill up with de-ionized to the
calibration mark. This corresponds to a concentration of 5 mL/L.
Standard Solutions:
Standard solutions with the following concentrations in water are prepared out of the stock solutions:
0.05 mL/L, 0.1 mL/L and 0.5 mL/L*
*The correct values have to be calculated out of the real initial weight and the content of Silverlume B Plus in
the certified reference.
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 e.g. 1:20 or 1:10.
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Evaluation:
Retention time:
Silverlume B Plus
approx. 1.0 min
The content of Silverlume B Plus is evaluated via linear external calibration. The content in mL/L is
calculated as follows.
Silverlume B Plus
Example:
Fig.1: Example chromatogram of a sample solution diluted 1:10.
0,110
0,100
0,090
0,080
0,070
AU
0,060
0,050
0,040
0,030
0,986
0,020
0,010
0,000
0,20
0,40
0,60
0,80
1,00
1,20
1,40
1,60
Minutes
1,80
2,00
2,20
2,40
2,60
2,80
3,00
*
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
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)
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.
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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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Reagents required*:
Sodium chloride
Silver nitrate solution 1 N (170 g/l AgNO3)
Be sure to observe all local regulations concerning the permitted limits for
pollutants, including the general regulations for hazardous materials!
Procedure:
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***
Example:
The following amount was used for the titration of 10.0 ml bath:
7.6 ml 0.5 n hydrochloric acid volumetric solution
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Calculation:
7.6 x 5.3 = 40.3 g/l sodium carbonate
7.6 x 6.9 = 52.4 g/l potassium carbonate
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:
12.6 ml 0.5 n hydrochloric acid volumetric solution
The following amount was used for titration after the addition of 1 m barium chloride solution:
5.0 ml 0.5 n hydrochloric acid volumetric 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
*
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: 02
Doc.-No.: EXT-0001-TIT-02
Principle:
Redox titration
Required reagents*:
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 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
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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,
The volume in ml of the 0.1 M Silver nitrate standard solution*** used for the titration of 2.5 ml sample,
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
*
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
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.
Be sure to observe all local regulations concerning the permitted limits for
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
*
**
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Version: 03
Doc.-No.: EXT-0346-TIT-03
Reagents required*:
Please follow the general regulations for hazardous materials in the Material safety
data sheets!
The analytical procedure is to be followed exactly.
Be sure to observe all local regulations concerning the permitted limits for
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.
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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
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.
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