EcoTri HC2 Ds v14
EcoTri HC2 Ds v14
Doc.-No.: 1035
DATA SHEET
SAP-No.: 1678479
CONTENTS
1. Process Information................................................................................................................................. 2
2. Equipment ............................................................................................................................................... 2
3. Cleaning Procedure for the Decontamination of Cr(VI)........................................................................... 3
4. Make-Up .................................................................................................................................................. 3
5. Working Parameters ................................................................................................................................ 4
6. Maintenance ............................................................................................................................................ 4
7. Control of the Cr (III) Content .................................................................................................................. 5
8. Control of the pH ..................................................................................................................................... 5
9. Guidelines for the Storage of EcoTri HC2 concentrate ........................................................................... 5
10. Application Guidelines ............................................................................................................................. 6
11. SAP No. for Make - Up and Maintenance Products ................................................................................ 6
12. General Safety Precautions .................................................................................................................... 6
13. Recommendations for Wastewater Treatment ........................................................................................ 7
14. Analytical Instructions .............................................................................................................................. 8
Determination of EcoTri HC2 by Photometry ..................................................................................... 8
Determination of Cr(III) by Titration ..................................................................................................10
Determination of Chromium(VI) by Photometry ...............................................................................13
Determination of Zinc by F-AAS .......................................................................................................15
Determination of Iron by F-AAS .......................................................................................................18
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1. Process Information
• EcoTri HC2 is a Chromium(III) containing thick layer passivation for zinc and zinc alloy which is
completely free of Chromium(VI).
• With EcoTri HC2 excellent corrosion resistance can be achieved which corresponds to a Cr(VI)
containing yellow chromate.
• Especially when heat treatment is required prior to corrosion testing (e.g. 1 hour at 120 °C,
2 hours at 180 °C, 24 hours at 120 °C) the corrosion protection is excellent.
• EcoTri HC2 produces green-red iridescent passivate layers on all kind of zinc surfaces with an
increased passivation layer thickness compared to an usual blue passivation.
• EcoTri HC2 can be used for both rack and barrel plating.
2. Equipment
Heating Required
Heater or heat exchanger made of PTFE.
Filtration Required
Exhaust Required
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If a customer wants to use an old tank, which until now was used for Cr(VI) containing chromates, the
customer is obliged to decontaminate the tank before using trivalent passivate solutions in the same tank.
It should be recognized that it is difficult to remove all traces of hexavalent chromium and all tanks and
ancillary equipment should be washed down and cleaned by hand, scrubbing or power washing might be
needed.
After cleaning and leaching the tanks they should be filled with clean water and tested for the presence of
Cr(VI). The according analytical method can be found in the last chapter of this document.
Note: The bisulfite solution can be used afterwards for waste treatment of Cr(VI) solutions.
4. Make-Up
The pH must be adjusted to working range with nitric acid or sodium hydroxide!
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5. Working Parameters
pH
zinc zinc iron zinc nickel
For use on zinc prior to passivation with EcoTri HC2 it is recommended to use either a hydrochloric acid or a
nitric acid dip (0.3 % (v/v)). We advise to use three rinsing tanks equipped with spray bars after the
passivation with EcoTri HC2.
6. Maintenance
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8. Control of the pH
After addition of EcoTri HC2 the pH must be checked and if necessary adjusted with NaOH
or HNO3.
EcoTri HC2 concentrate should be stored at normal indoor conditions. The recommended temperature
range is 8 – 30 °C.
Do not store EcoTri HC2 concentrate for extended period at temperatures above 40 °C or below 0 °C. This
can lead to a shorter shelf life or to freezing of the product.
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• Generally, the high working temperature causes the high corrosion resistance.
Therefore avoid using a low working temperature.
• Higher temperatures and a lower pH need shorter immersion times.
• Lower temperatures and a higher pH need longer immersion times.
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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Concentrates should be diluted with the rinse water in the ratio of 1 : 3 and then neutralized with calcium
hydroxide (Ca-lime) to pH 10 and a minimum reaction time of 1 h.
For better flocculation add flocculation agent (recommended is polyacryl amide/anionic with a molecular
weight of 4 - 6 million) and stir. Allow the precipitate to settle for better filtration.
After filtration is complete the filtrate must not be mixed with metal ions bearing waste streams.
Be sure to observe all local regulations concerning the limit values of pollutants
including the general regulations on dangerous materials!!
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Version: 01
Determination of EcoTri HC2 by Photometry
Doc.-No.: EXT-0879-UV-01
Principle:
At 560 nm, Cr(III) shows an extinction maximum that is used for the quantitative determination.
Reagents required*:
Be sure to observe all local regulations concerning the permitted limits for
pollutants, including the general regulations for hazardous materials!
Equipment required:
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Procedure:
A) Calibration Solutions (Standards):
• 10.0** ml of each of the stock solutions are pipetted into separate 50 ml volumetric flasks, 5ml 5M Nitric
Acid is added into each and then filled up to the mark with DI Water.
Evaluation:
Determination of the content of EcoTri HC2 of the sample to be analyzed is carried out by comparing the
extinction result with the calibration graph previously plotted or calculation.
Example:
Extinctions of the calibration solutions: 100 ml/l: E100 = 0.103; 120 ml/l: E120 = 0.124; 140 ml/l: E140 = 0.145.
Extinction sample: Esample = 0.133.
Calculation:
Quality assurance: For maintenance, calibration of measuring devices and the use of
standards and reference materials please refer to the corresponding guidelines.
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Version: 03
Determination of Cr(III) by Titration
Doc.-No.: EXT-0858-TIT-03
Reagents required*:
Be sure to observe all local regulations concerning the permitted limits for
pollutants, including the general regulations for hazardous materials!
The sample amounts and factors given in the table below can be used for most of the passivations.
<2 10 0.173
2-5 5 0.346
5-10 2 0.867
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Procedure:
• Place sample (refer table above) into a 250 ml Erlenmeyer flask and mix with
• 2 ml sodium hydroxide solution 5 M,
• 50 ml DI water.
• Carefully add 20 ml hydrogen peroxide 30% (in portions) and cover the flask with a funnel.
• Allow boiling for 20-30 min (the hydrogen must be boiled down completely!).
• After the solution cooled down to 60-80°C, add
• 10 ml hydrochloric acid conc. and
• 10 ml phosphoric acid conc.
• Cool down to room temperature (not necessary if you work without the indicator on an titroprocessor)
and fill up to 100 ml with DI water.
• After addition of 4 drops indicator titrate with
• 0.1 M Ammonium iron(II) sulfate volumetric solution until the deep violet colour of the solution changes
to a light green/yellow.
Calculation:
•
The amount of ml of 0.1 M Ammonium iron(II)-sulfate volumetric solution used – multiplied by the factor
indicated in the table above – gives the content of Cr(III) in g/l.
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Example:
1. Example
During titration of 2.0 ml sample, 11.2 ml of of 0.1 M Ammonium iron (II) sulfate volumetric solution was
used.
2. Example
During titration of 5.0 ml sample, 13.2 of 0.1 M Ammonium iron (II) sulfate volumetric solution was used.
3. Example
During titration of 10.0 ml bath, 6.6 ml of of 0.1 M Ammonium iron (II) sulfate volumetric solution was used.
Quality assurance: For maintenance, calibration of measuring devices and the use of
standards and reference materials please refer to the corresponding guidelines.
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Version: 07
Determination of Chromium(VI) by Photometry
Doc.-No.: A0000389-07
Reagents required*:
• Reagent 1:
700 ml phosphoric acid will be filled with water to 1000 ml
• Reagent 2:
1 g of 1.5-Diphenylcarbazide dissolved in 100 ml acetone and acidified with a drop of conc acetic acid.
• Cr(VI) stock solution, 1.0 g/l: 2829 mg potassium dichromate will be dissolved in DI water and topped
up to 1000 ml using a volumetric flask.
• Cr(VI) standard solution 1.0 mg/l: 1.0 ml of Cr(VI) stock solution are pipetted into a 1000 ml
volumetric flask and filled up with 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:
Parameters
Methode Cr VI
Curve linear
Wavelength 540 nm
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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Procedure:
•
6+
Due to the inherent color of the sample it is necessary to fix the LOQ of the method to 1.0 mg/l Cr .
Evaluation:
The content of Cr(VI) in the sample is evaluated by standard addition method. The result is given in
mg/l.
Quality assurance: For maintenance, calibration of measuring devices and the use of
standards and reference materials please refer to the corresponding guidelines.
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Version: 02
Determination of Zinc by F-AAS
Doc.-No.: EXT-0175-AA-02
Principle:
The solution will be atomized and afterwards the extinction will be measured in an air/acetylene flame at the
corresponding wavelength. Evaluation is carried out by an external calibration using aqueous standard
solutions.
Reagents required*:
Be sure to observe all local regulations concerning the permitted limits for
pollutants, including the general regulations for hazardous materials!
Equipment required
• Atomic absorption spectrometer (2100/4100 with control and evaluation unit, e.g.
Messrs. Perkin Elmer or equivalent type)
• Burner: air/acetylene single-slit burner head (e.g. Messrs. Perkin Elmer)
• Heater plate
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Standards:
0.5 mg/l Zn: 0.25 ml of zinc standard solution and 5 ml of 5 M nitric acid are to be pipetted into a 500 ml
flask then filled up to the mark with DI water and mixed thoroughly.
1.0 mg/l Zn: 0.50 ml of zinc standard solution and 10 ml of 5 M nitric acid are to be pipetted in to a 500 ml
flask then filled up to the mark with DI water and mixed thoroughly.
Operating conditions:
Varian AA280FS
Please consult the instruction manual provided by the manufacturer of the AAS
system, for information on the individual parameters such as the flame, the slit
width, the integration period, etc.
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Procedure
•
**
1.0 ml sample are pipetted into a 50 ml volumetric flask. After addition of
• about 2 ml nitric acid it will be topped up to the required level with DI water and mixed thoroughly
(dilution factor = 50).
• For determination of the zinc content, this solution must be further diluted in a ratio of
1 : 500 with DI water prior to measurement (dilution factor = 25,000)
For the operational range please refer to the Datasheet and chose dilution accordingly!
If the sample absorbance is out of the calibrated range another dilution has to be chosen!
Evaluation
Example:
Calculation:
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Version: 02
Determination of Iron by F-AAS
Doc.-No.: EXT-0176-AA-02
Principle:
The solution will be atomized and afterwards the extinction will be measured in an air/acetylene flame at the
corresponding wavelength. Evaluation is carried out by an external calibration using aqueous standard
solutions.
Reagents required*:
Be sure to observe all local regulations concerning the permitted limits for
pollutants, including the general regulations for hazardous materials!
Equipment required
• Atomic absorption spectrometer (2100/4100 with control and evaluation unit, e.g.
Messrs. Perkin Elmer or equivalent type)
• Burner: air/acetylene single-slit burner head (e.g. Messrs. Perkin Elmer)
• Heater plate
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Operating conditions:
Varian AA 280FS
Please consult the instruction manual provided by the manufacturer of the AAS
system, for information on the individual parameters such as the flame, the slit
width, the integration period, etc.
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Calibration
The dilution ratio depends on the iron or zinc concentration of the solution to be analyzed. Due to the
influence of the matrix, however, the solution must be diluted at a ratio of at least 1 : 10 in any case. With
„normal“ working conditions the following dilution ratios are recommend:
Determination of Iron 1 : 25 to 1 : 50
•
**
1.0 ml sample are pipetted into a 50 ml volumetric flask. After addition of
• about 2 ml nitric acid it will be topped up to the required level with DI water and mixed thoroughly
(dilution factor = 50).
• It is now possible to directly determine the iron content by AAS without further dilution.
For the operational range please refer to the Datasheet and chose dilution accordingly!
If the sample absorbance is out of the calibrated range another dilution has to be chosen!
Evaluation
Example
Calculation
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
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