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ChromKlad™ 2500

Hard Chromium Plating Process


#171191

Europe
Technical Data Sheet

Table of Contents:

1. Process Description & Advantages

2. Deposit Properties

3. Process Components

4. Bath Make-Up

5. Bath Operation & Control

6. Solution Analysis

7. General Guidelines

8. Addition Tables

9. Waste Management

10. Safety & Handling Guidelines

11. Ordering Information

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 2

1. Process Description & Advantages

Description
The MacDermid ChromKlad™ 2500 is an efficient industrial (hard) chromium
plating process which utilizes a non-halogen catalyst system.

Advantages
z Improved efficiency over conventional systems
z Free of fluorides and other halogens
z Hard deposit (1100-1250 HV100)
z Micro-cracked deposit (> 400/cm)
z Bright deposit
z Improved deposit uniformity, particularly when compared to sulfate-
fluoride type chemistries.
z Uses standard pretreatment and anodes

Feature Benefit

Considerable reduction in plating time


Improved efficiency Increased production per tank
Significant reduction in overall operating cost

Reduced plating times to achieve thickness


Improved uniformity Reduced machining after plating
Less chromium wasted on over plated HCD areas

Hard deposit (1100-1250 HV100) Improved resistance to abrasion wear


Improved corrosion resistance
Micro-cracked deposit
Small cracks hold oil and lubricate mating surfaces

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 3

2. Deposit Properties
Property Typical Value
Density 6.9 g/cm3
Micro-cracks > 400/cm
Hardness 1,100 – 1,250 HV100 (as plated)

3. Process Components

Make-Up Components: Europe


Concentration
ChromKlad 2500 Make Up Salt (71191) 250 g/L
ChromKlad 2500 Catalyst (71193) 50 mL/L

Replenishment Components Options:


Solid Replenishment Option 1:

ChromKlad™ 2500 S Maint Salt (71195) compound is a solid replenishment


component added to the bath to maintain the proper concentration of chromic
acid and secondary catalyst in solution. This compound is replenished based on
analysis of the chromic acid concentration at a rate of 1.5 kg per 10,000 ampere-
hours.

Liquid Replenishment Option 2:

ChromKlad™ 2500 LC Maint Soln (71185) is a liquid replenishment component


added to the bath to maintain the proper concentration of chromic acid and
secondary catalyst in solution. ChromKlad™ 2500 LC Maint Soln contains 300
g/L of chromic acid in order to comply with European regulations for shipment of
hazardous materials. This liquid maintenance chemistry is replenished based on
analysis of the chromic acid concentration at a rate of 500 mL per 1,000 ampere-
hours.

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 4

ChromKlad™ 2500 Catalyst (71193) can be added, when needed, to adjust the
concentration of active catalyst in the bath. Additions of this chemistry should
only be made to the bath on recommendations from the MacDermid customer
service laboratory, after analysis of the solution chemistry.

Sulfuric acid should be used to maintain the primary catalyst in solution. (See
table II for recommended additions).

4. Bath Make-Up
To Make-Up The Bath:
Tank Preparation
Thoroughly clean the plating tank, anodes and heating coils. Remove all sludge
and repair any holes in the tank lining. Anodes should be cleaned using
ChromKlad Anode Cleaner (71175), then returned to the tank after thorough
rinsing.

Make-up Procedure
1. Fill the thoroughly cleaned tank to 1/2 of its final volume with deionized
water and heat to 66ºC. If deionized water is not available, check water
for chloride contamination, using the procedure for the Determination of
Chloride found in the Solution Analysis section of this technical data sheet.
If the water is high in chloride (> 20 ppm), consult your MacDermid
representative for specific recommendations for removing chloride using
silver oxide (Ag2O).
2. While the hot water is being agitated, using either a low pressure blower or
mechanical agitation, slowly add the calculated amount of ChromKlad™
2500 Make Up Salt. The agitation should be continued until all of the salts
have been dissolved. Slowly add the calculated amount of ChromKlad™
2500 Catalyst to the tank. After all of these additions have been made,
the tank volume should be adjusted to its final operating level with water.
3. Adjust the temperature of the solution to operating range, 60ºC, and
dummy the bath at plating current density for several hours.
4. After the initial electrolysis of the solution, the bath is ready for production
plating.

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 5

5. Bath Operation & Control


The operating parameters for the ChromKlad™ 2500 system are as follows:
Parameter Range Target
Chromic Acid: 210-285 g/L 250 g/L

Ratio (CrO3/SO4): 80 to 100:1 90:1

Temperature: 54-66ºC 60ºC

Cathode Current Density: 16-93 ASD (1.0-6.0 ASI)

8-47 ASD (0.5-3.0 ASI)


Anode Current Density:

Equipment

Plating Tank: Flexible polyvinyl chloride,


such as Koroseal or equivalent

Anodes: 7% Tin/Lead anodes or Platinised Titanium

Heating/Cooling Coils: Titanium, PTFE or similar fluorocarbon polymer coils

Power Supply: D.C. power supply (9-15 volts)


with less than 5% ripple

Agitation: Low pressure blower

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 6

6. Solution Analysis
Chromic acid concentration can be estimated with a hydrometer, however, it is
recommended that periodic chemical analysis for the ChromKlad™ 2500 be
made. Baumé readings should be made at least daily to determine the
ChromKlad™ 2500 content of the solution. When the chromic acid concentration
drops below 250 g/L ChromKlad™ 2500 S Maint Salt or 2500 LC Maint Soln
should be added to bring the solution back to this concentration. An addition of
about 11.44kg/100L will raise the concentration of the solution approximately 1º
Baumé. Chemical analysis can be used to determine the concentration of
chromic acid in the bath and these results compared to the Baumé readings. If
the Baumé reading indicates more ChromKlad™ 2500 than is shown by analysis,
metallic contamination is present. Most metallic contamination only increases the
resistance of the bath to current flow, and gives false high Baumé readings. The
Baumé readings may then be adjusted to give true readings.

The sulfate may be checked using a Kocour sulfate test kit. If the sulfate is low,
66º Baumé sulfuric acid can be added at the rate of 4.1 mL/100L of the solution
to raise the sulfate 0.075 g/L. If the sulfate is too high, barium carbonate can be
added at the rate of 0.15 g/L to reduce the sulfate 0.075 g/L. Barium carbonate,
when added to a chrome plating solution, forms barium sulfate and barium
chromate. Thus, as time passes, the barium chromate slowly decomposes and
forms barium sulfate. This process may take as long as 24 hours. Thus, an
addition of barium carbonate may not give the full response desired, immediately.
It is also better to divide the entire amount of barium carbonate to be added into 4
lots, and add one lot every two hours while no work is in the tank. The dry
barium carbonate may be sprinkled over the surface of the chrome solution, or a
slurry mixture of the barium carbonate in water may be slowly poured into the
chrome solution. A thorough mixing of the chrome solution should follow these
additions.

Determination Of Chromium
Reagents required:

– C.P. Grade Hydrochloric Acid (HCL)


– Ammonium Bifluoride (NH4HF2)
– 10% Potassium Iodide (KI)
– Standardized 0.1N Sodium Thiosulfate (Na2S2O3)
– Starch Solution (4 g/L soluble starch) or Thyodene

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 7

Method for analysis of ChromKlad ™ 2500

1. Pipette a 5 mL sample of the ChromKlad™ 2500 solution into a 250 mL


volumetric flask, dilute to mark with distilled water and mix thoroughly.
2. Pipette 10 mL of the solution from the volumetric flask into a 250 mL
Erlenmeyer flask.
3. Dilute to about 100 mL with distilled water.
4. Add 15 mL of concentrated hydrochloric acid and mix.
5. Add about 2 grams of ammonium bifluoride. Swirl the solution until the
bifluoride is dissolved.
6. Add 10 mL of a 10% potassium iodide solution.
7. Immediately titrate with 0.1 N sodium thiosulfate until the dark brown solution
fades to a light straw color.
8. Add about 5 mL of starch indicator solution or 0.1 g thyodene. The solution
should turn dark blue to purple. Continue titrating with the thiosulfate solution
until the color fades to a light green blue color. This color should hold for at
least a minute if the endpoint has been reached. If it turns dark in less than a
minute, another drop or two of the thiosulfate is needed.
9. Calculate the chromic acid concentration:

Chromic acid (g/L) = mL of 0.1 N sodium thiosulfate solution used X 16.67

Determination Of Sulfate

Recommend use of Kocour Centrifuge method for determination of sulfate.

Determination Of Active Catalyst

Submit sample of ChromKlad™ 2500 solution to the nearest MacDermid


customer service laboratory for determination of active catalyst.

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 8

Determination Of Trivalent Chromium

Reagents Required:

– Sodium Peroxide (Na2O2)


– Ammonium Bifluoride (NH4HF2)
– C.P. Grade Hydrochloric Acid (HCL)
– 10% Potassium Iodide (KI)
– Standardized 0.1N Sodium Thiosulfate (Na2S2O3)
– Starch Solution (4 g/L soluble starch) or Thyodene

Method of Analysis for Trivalent Chromium

1. Pipette a 5 mL sample of the ChromKlad™ 2500 solution into a 250 mL


volumetric flask, dilute to mark with distilled water and mix thoroughly.
2. Pipette 10 mL of the solution from the volumetric flask into a 250 mL
Erlenmeyer flask.
3. Dilute to about 125 mL with distilled water.
4. Add about 0.2 grams of sodium peroxide.
5. Place flask on hot plate and boil for no less than 20 minutes and no more
than 30 minutes.
6. Dilute to about 125 mL with distilled water and allow to cool.
7. Add about 2 grams of ammonium bifluoride. Swirl the solution until the
bifluoride is dissolved.
8. Add 15 mL of concentrated hydrochloric acid and mix.
9. Add 10 mL of a 10% potassium iodide solution.
10. Immediately titrate with 0.1 N sodium thiosulfate until the dark brown
solution fades to a light straw color.
11. Add about 5 mL of starch indicator solution or 0.1 g thyodene. The
solution should turn dark blue to purple. Continue titrating with the
thiosulfate solution until the color fades to a light green blue color. This
color should hold for at least a minute if the endpoint has been reached. If
it turns dark in less than a minute, another drop or two of the thiosulfate is
needed.
12. Calculate the trivalent chromium (Cr3+) concentration:

Trivalent Chromium (g/L) =


(mL 0.1N Na2S2O3 – 0.1 N Na2S2O3 from CrO3 titration) X 8.78

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 9

Trivalent chromium is constantly being generated in the bath as a by product of


the reaction which reduces Cr6+ to chromium metal, however, the concentration
of trivalent chromium in the bath should reach an equilibrium in solution and
stabilize. An increase in the concentration of trivalent chromium in the bath
indicates 1) there is insufficient anode area in the bath or 2) organic
contamination of the solution. The concentration of trivalent chromium should not
be allowed to exceed 3.75 g/L. Trivalent chromium is removed from a solution of
ChromKlad™ 2500 the same way you remove trivalent chromium from any
chrome plating solution. Electrolyze the solution at 6 volts, using high anode
area and low cathode area (30:1 ratio of anode to cathode is optimum). It is
possible to remove 7.5g/L of trivalent chromium from a solution of ChromKlad™
2500, under optimum conditions (30:1 anode to cathode ratio, 6 volt potential, at
54ºC) in 12 hours.

Determination Of Chloride

Reagents Required:

⎯ 1:1 Nitric Acid


⎯ 0.1 N Silver Nitrate (AgNO3) Solution
⎯ 0.01 N Mercuric Nitrate Solution—Dissolve 1.083 grams mercuric
oxide in 5 mL of 50% Nitric Acid. Dilute to 1 liter with Distilled
water. This solution does not need to be standardized.

Method for Analysis of Chloride

1. Pipette a 5 mL sample of the ChromKlad™ 2500 solution into a 100 mL


beaker that has been rinsed with distilled water.
2. Add a magnetic stirring bar that has also been rinsed with distilled water.
3. Add 20 mL of 1:1 nitric acid solution.
4. Dilute to about 100 mL with distilled water.
5. Place beaker on a stir plate and note the clarity of the solution while
looking through it.
6. Add 3 drops of 0.1 N Silver Nitrate (AgNO3) Solution.
7. Titrate using 0.01 N Mercuric Nitrate from turbid to clear.
8. Calculate the chloride concentration:

Chloride (ppm) = (mL 0.01 N Mercuric Nitrate) X 71

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 10

7. General Guidelines

Troubleshooting Guide
A ChromKlad™ 2500 troubleshooting guide can be obtained from your local
MacDermid field representative.

Bath Conversions
Most hard chromium plating solutions can easily be converted to ChromKlad™
2500. A 1 liter sample of the current plating solution should be send to the
nearest MacDermid Customer Service Plating Laboratory for specific
recommendations on conversion procedures.

Mist Suppressant
ChromKlad MS (71179) can be used to eliminate chromium mist from the
ChromKlad™ 2500 solution. ChromKlad MS is a stable, highly effective liquid
wetting agent for reducing the surface tension of hard chromium plating solutions
to meet the current EPA and AQMD Rule 1469(c)(14) requirements. Use of
ChromKlad MS also reduces drag-out losses of the plating solution, reduces
contamination of adjacent plating operations, and reduces maintenance
requirements of ventilation equipment.

Equipment
Existing equipment may be satisfactory for the use of the ChromKlad™ 2500
process. If there is any doubt, the following discussion may prove helpful.

Plating Tank
Approved plastic lined tanks are recommended, flexible polyvinyl chloride, such
as Koroseal or equivalent.

Anodes
The use of 7% Tin/Lead anode material is recommended although it is possible
to use platinised tintanium if required. Solid round anodes have been found to
give the least trouble and the longest life. They should be of sufficient cross
sectional area to conduct the required current without over-heating the anode.
The anode area should be 1½ times the cathode area.
If the anodes become coated with an orange-yellow lead chromate scale they
should be cleaned using ChromKlad Anode Cleaner (71175).

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 11

Associated Equipment
The tank should be supplied with venting equipment, heating and cooling coils,
and automatic temperature controls. The heating-cooling coils may be made of
titanium, PTFE or similar fluorocarbon polymer coils. The bus bars and anode
bars should be adequate to carry the current without over heating. All conducting
materials, except the bus bars, associated with the tank, should be insulated from
external sources of power to prevent stray currents.
Since a homogenous solution is desired, some means of preventing stratification
is required, such as pumping the solution or using a low pressure air blower.

Power Supply
The power supply may be either a rectifier or a generator which can supply up to
800 ASF (6 ASI) at 9-12 volts, with a recommended ripple characteristic of less
than 5% at any setting. Larger installations may require up to 15 volt potential. If
the power supply is in doubt, consult your MacDermid representative. All current
carrying members of the system must be adequate to carry the calculated current
without over-heating.

8. Addition Tables
The level of the plating solution should be maintained by additions of clean water
from an uncontaminated drag-out tank. In addition to maintaining the correct level
in the tank, the solution should be thoroughly stirred before measuring its density
or taking a sample. Any decrease in density from the recommended value should
be corrected by the addition of ChromKlad™ 2500 S Maint Salt or 2500 LC Maint
Soln. The following table can be used as a guide.

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 12

Table I
Density of ChromKlad™ 2500 Solution
CrO3 Specific Gravity Degrees Baumé Degrees Baumé
oz/gal g/L 15ºC (60ºF) 15ºC (60ºF) 54ºC (130ºF)
25.0 187.5 1.1328 17 15.6
26.7 200.0 1.1417 18 16.8
28.5 213.8 1.1508 19 17.9
30.0 225.0 1.1600 20 18.6
32.2 241.5 1.1694 21 19.5
34.1 255.8 1.1789 22 20.7
36.0 270.0 1.1885 23 21.7
37.9 284.3 1.1983 24 22.9
39.8 298.5 1.2083 25 23.4
41.8 313.5 1.2185 26 24.5
43.9 329.3 1.2288 27 25.5
46.0 345.0 1.2393 28 26.5
48.2 361.5 1.2500 29 27.4
50.3 377.3 1.2609 30 28.6
52.5 393.8 1.2719 31 29.8
54.8 411.0 1.2832 32 31.0

TABLE IIA
Amount of Sulfuric Acid Required to Increase Sulfate
Milliliters of 66º Baumé Sulfuric Acid (Specific Gravity = 1.84) Required
SO4 (g/L) Tank Volume
to be added 100 Liters 200 Liters 500 Liters 1,000 Liters
0.1 5.9 11.8 29.5 59.0
0.2 11.8 23.6 59.6 118.0
0.3 17.9 35.8 89.5 179.0
0.4 23.8 47.6 119.0 238.0
0.5 29.5 59.0 147.5 295.0
0.6 35.4 70.8 177.0 354.0
0.7 41.3 82.6 206.5 413.0
0.8 47.2 95.4 236.0 472.0
0.9 53.1 106.2 265.5 531.0
1.0 59.0 118.0 295.0 590.0

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 13

Table IIIA
Amount of Barium Carbonate (Grams) Required to Lower Sulfate
SO4 (g/L) Tank Volume
to be removed 100 Liters 200 Liters 500 Liters 1,000 Liters
0.1 20.0 40.0 100.0 200.0
0.2 40.0 80.0 200.0 400.0
0.3 60.0 120.0 300.0 600.0
0.4 80.0 160.0 400.0 800.0
0.5 100.0 200.0 500.0 1000.0
0.6 120.0 240.0 600.0 1200.0
0.7 140.0 280.0 700.0 1400.0
0.8 160.0 320.0 800.0 1600.0
0.9 180.0 360.0 900.0 1800.0
1.0 200.0 400.0 1000.0 2000.0

9. Waste Management
Solutions of ChromKlad™ 2500 are acidic and contain chromic acid. This
solution must not be discharged directly into a sewage system without proper
treatment according to local/state/federal regulations.

Specific options for management of waste can be obtained through your local
MacDermid, Inc. representative. However, prior to using any recommendations
or suggestions by MacDermid, Inc. for waste treatment, the user is required to
know the appropriate local/state/federal regulations for on-site or off-site
treatment, which may require permits. If there is any conflict regarding our
recommendations, local/state/federal regulations take precedence.

10. Safety & Handling Guidelines

Caution
Store all ChromKlad™ 2500 chemistry in tightly closed containers at temperature
above 10°C (50°F). Storage temperatures should not exceed 38°C (100°F).
Avoid contact with eyes, skin and clothing.

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 14

Protective Equipment
When handling liquid concentrates and solutions, wear rubber gloves, safety
glasses and chemical-resistant apron. Wash thoroughly after handling. The area
immediately around the plating tank must be ventilated.

First Aid
In case of eye or skin contact, immediately flush with large amounts of water for
at least 15 minutes. For eye contact, immediately call a physician. If swallowed,
immediately call a physician.

Spill Or Leak
Wear protective equipment during clean up. Absorb spill or leak with an inert
material such as sand, earth or vermiculite. Dispose of absorbing material
according with local/state/federal regulations.

ChromKlad™ 2500 CHEMISTRY is for industrial use only.


Read Material Safety Data Sheets and product labels before use.

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com
ChromKlad™2500 #171191 Page 15

11. Ordering Information

Product Name / Function Product Code

ChromKlad™ 2500 Make Up Salt 71191


ChromKlad™ 2500 Catalyst 71193
ChromKlad™ 2500 S Maint Salt 71195
ChromKlad™ 2500 LC Maint Soln 71185
ChromKlad MS 71179
ChromKlad AC 71175

Revised Version 2.2


February 2009

Also read carefully warning and safety information on the Material Safety Data Sheet. This data sheet contains technical information
required for safe and economical operation of this product. READ IT THOROUGHLY PRIOR TO PRODUCT USE. Emergency directory
assistance Chemtrec 1-800-424-9300.
DISCLAIMER: All statements, technical information and recommendations contained herein are based on tests we believe to be reliable, but
the accuracy or completeness thereof is not guaranteed. No statement or recommendation shall constitute a representation unless set forth
in an agreement signed by officers of seller and manufacturer. NO WARRANTY OR MERCHANTABILITY OR WARRANTY OF FITNESS
FOR A PARTICULAR PURPOSE IS MADE. The following warranty is made in lieu of such warranties and all other warranties, express,
implied, or statutory.
Products are warranted to be free from defects in material and workmanship at the time sold. The sole obligation of seller and manufacturer
under this warranty shall be to replace any product defective at the time sold. Under no circumstances shall manufacturer or seller be liable
for any loss, damage or expense, direct or consequential, arising out of the inability to use the product.
Notwithstanding the foregoing, if products are supplied in response to a customer request that specifies operating parameters beyond those
stated above, or if products are used under conditions exceeding said parameters, the customer by acceptance or use thereof assumes all
risk of product failure and of all direct, indirect and consequential damages that may result from use of the products under conditions, and
agrees to exonerate, indemnify and hold harm Less MacDermid Incorporated there from.
No suggestion for product use nor anything contained herein shall be construed as a recommendation to use any product in infringement of
any patent rights, and seller and manufacturer assume no responsibility or liability for any such infringement.

MacDermid plc, 198 Golden Hillock Road, Birmingham B11 2PN, England
International Telephone: + 44 (0) 121 606 8100 Fax: + 44 (0) 121 606 8300
www.macdermid.com

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