Technical Q & A

Columbia Chemical Technical Support Representatives can be contacted at 330/225-3200 or techsupport@columbiachemical.com.

 

Plating Alkaline Non-Cyanide Over High Carbon or Heat-Treated Substrates

Standardized Pretreatment Guidelines for Passing the Nitric Acid Test with Marquee Electroless Nickel Over Zinc Die Cast and Aluminum Substrates

Key Indicators of Lead Contamination

Recommendations for Reducing Hex-chrome Contamination

Removing Carbon from Steel Prior to Zinc Plating

Processing High Carbon and Heat-treated Steel in an Alkaline non-Cyanide Zinc Process

Acid Chloride Zinc Post-Plate Staining

Alkaline Non-cyanide Poor Cathode Efficiency

Staining Problems in Acid Zinc: Low Cloud Point

Rack Marks on Tubes in Alkaline Zinc

Dull Alkaline Zinc Deposits: Organic Contamination

 


 

Plating Alkaline Non-Cyanide Over High Carbon or Heat-Treated Substrates

Question:  We are having major issues with zinc adhesion and corrosion failures with a heat-treated fastener.  The problem is not being seen on all work going through the line, only on this one specific piece.

Our pre-treatment sequence is the same for every job and is described below.

  1. Hot alkaline soak, 160°F, 15 to 20 Minutes
  2. Rinse
  3. Hydrochloric acid pickle, 25% by volume – 15 to 20 minutes
  4. Rinse
  5. Hot alkaline electro, 160°F - 5 to 10 minutes
  6. Rinse
  7. Caustic soda rinse
  8. Plate (Alkaline Non-Cyanide)

The plating bath does appear to be in relatively good shape, no other parts are seeing corrosion failures or adhesion issues.

Do you have any suggestions? 

Answer:  The information you supplied indicates that the heat treated fasteners are being over exposed to the pretreatment chemistries. 

The recommended sequence and times are as follows:

1. HOT ALKALINE SOAK CLEANER - Oil removal / Organic removal - Any oily material was found on the surface of the substrate, even if fastener does not appear to be heavily oiled and confirmed, will need to be pass through a hot alkaline soak cleaner.  This will remove the lubricating oils used during manufacturing allow the substrate to be effectively pre-treated in the hydrochloric acid pickle.  It is highly recommended reducing the time within the hot alkaline soak cleaner to 5 to 10 minutes. 

2.  Rinses

3.  HYDROCHLORIC ACID PICKLE - Scale removal / Red rust removal – Excessive scale or corrosion will need to be removed.  Due to the nature of your substrate, hardened/heat-treated, it will be extremely important to NOT over acid pickle the pieces.  Excessive exposure to high concentrations of hydrochloric acid or high dwell times in the acid pickle will produce a very heavy layer of inert carbon.  The carbon layer will interfere with the appearance, adhesion and performance of the zinc deposit/chromate layer, especially when processing through an alkaline non-cyanide electrolyte.

a.  It is highly recommended adding 2% by volume PICKLE PAL or PICKLE PAL PLUS to the hydrochloric acid pickle.  PICKLE PAL and PICKLE PAL PLUS are formulated to greatly reduce the acid etch of the steel substrate.

b.  It is highly recommended reducing the overall time.  Maintain exposure time at 5 to 10 minutes.

c.  If acid pickle is not effective at removing the heavy scale, increasing the acid concentration to 30 to 40% by volume is recommended.  NOTE: The use of PICKLE PAL or PICKLE PAL will allow for higher concentration of hydrochloric acid without acid etching of the steel substrate.

4.  Rinses 

5.  HOT ALKALINE ELECTRO-CLEANER - Carbon removal - The use of PICKLE PAL or PICKLE PAL PLUS will greatly reduce the carbon formation on the surface of the substrate, but the use on an anodic electro cleaner will still need to be used.  Alkaline cyanide free plating processes do not readily plate or adhere over the inert carbon surface.  Maintaining adequate current flow is critical, excessive current can case a degradation of the substrate resulting in a contaminated surface.

The above pretreatment cycle can be implemented immediately to ensure  the quality of the zinc and chromate films.  When processing heat-treated or hardened substrates, pretreatment is critical for the overall success and performance of the coatings applied.

 

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Standardized Pretreatment Guidelines for Passing the Nitric Acid Test with MARQUEE Electroless Nickel Over Zinc Die Cast and Aluminum Substrates

Question:  Is it possible to plate zinc die cast and aluminum substrates with your MARQUEE HP Electroless Nickel process and pass the nitric acid test?

Answer:  Columbia Chemical’s MARQUEE HP, our high phosphorus electroless nickel process, will pass the standard 30 second nitric acid dip test with no discoloration.  Optimized pretreatment cleaning of both substrates is critical to the overall consistency of your test results. 

Please review the below standardized pretreatment guideline for aluminum and zinc die cast substrates.

ZINC DIE CAST *

  1. Caustic Soak Cleaner
  2. Caustic Electro cleaner - Anodic
  3. 0.5%/wt sulfuric acid dip
  4. CuCN Strike
  5. Nickel Strike
  6. Electroless Nickel

* Detailed information can be found in the ASTM B 252-92 Preparation of Zinc Alloy Die Castings for Electroplating and Conversion Coatings specification. 

ALUMINUM *

  1. Caustic Soak Cleaner
  2. Alkaline Etch
  3. Rinse
  4. De-smut – Nitric acid/ammonium biflouride
  5. Zincate
  6. Zincate Strip
  7. Zincate
  8. Electroless Nickel

* Detailed information can be found in the ASTM B 253-87 Preparation of Aluminum Alloys for Electroplating specification. 

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Key Indicators of Lead Contamination

Question:  What is the indicator that we can see on the part if the alkaline non-cyanide solution is contaminated with lead.  Also, what is the minimum concentration of lead?  How can we remove lead contamination in an alkaline non-cyanide zinc solution?

Answer:  Lead contamination will have an overall dark/iridescent appearance after the chromate is applied. It is not recommended operating the process with contamination levels over 5 mg/L.

Treat plating solution with 1 pound zinc dust per 1,000 gallons of plating solution. Spread the zinc dust evenly over the entire surface of the plating solution and allow to mix a minimum of 1 hour. It is not recommended treating the bath during operation; the zinc dust will cause roughness.  Five micron filtration with a minimum bath turn-over-rate of twice per hour is recommended after the treatment is completed. 

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Recommendations for Reducing Hex-chrome Contamination

Question: I have a problem with chromium impurity in a non-cyanide alkaline zinc plating bath.  First, it was a blistered deposit, and now I have a black color at high current.  I am going to use sodium hydrosulfite.  For each 100 liters of bath I am going to use 8g of sodium hydrosulfite; dissolve the correct amount in warm water and immediately disperse throughout the zinc bath.  What do you think about this method?

Answer:  Hexavalent chrome contamination can be extremely detrimental to the overall appearance and adhesion of the zinc deposit. In most cases, the use of sodium bisulfite or sodium hydrosulfite can be used to reduce the hexavalent chrome into trivalent chrome. Hexavalent chrome contamination levels above 15 mg/L can simply stop production due to blistering and low current density skip plate. Below are typical treatments for reducing hexavalent chrome contamination:

  • Treat plating solution with 30 grams of sodium bisulfite per 1,000 liters of plating solution per 15 mg/L chrome contamination.
  • Treat plating solution with 15 grams of sodium hydrosulfite per 1,000

liters of plating solution per 15 mg/L chrome contamination.

I recommend that you measure out both the sodium bisulfite and sodium hydrosulfite and dilute with water prior to adding the working plating solution. The sodium bisulfite/sodium hydrosulfite solutions, with excellent agitation, can then be added evenly over the entire surface of the plating solution. This technique will ensure the entire plating solution is treated evenly.

These treatments are highly effective, but it is very important to eliminate the source of the hexavalent chrome contamination. This can be accomplished by improving or increasing pre-treatment rinse water flow rates and dumping and/or treating contaminated pre-treatment chemistry.

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Removing Carbon from Steel Prior to Zinc Plating

Question:  We are currently galvanizing on zinc-acid process in barrel iron castings which are machined. One of the biggest problems we have in cleaning is finding the middle ground that does not affect the machine against the areas where there is no machining. Due to the attack of the acid, which is added with inhibitors, we generated more coal on the surface, thus preventing adhesion of the coating. We have tried to follow the ASTM B-320 for best results, but the problem persists. Could you please offer a solution to this problem? Also, we would appreciate your advice with respect to the main problems associated with cleaning iron cast materials in zinc plating processes.

Answer:  Due to the high carbon content of iron castings, heat-treated and/or hardened components, optimum pre-treatment cleaning and sequencing is crucial to the overall performance of the finished coating. Carbon within these substrates will be pulled to the surface during scale removal or hydrochloric acid pickling. To reduce the acid etch on the steel, I suggest using an acid inhibitor. These inhibitors will allow the acid to remove the oxidized iron without pulling an excess amount of carbon to the surface.

Totally eliminating the formation of carbon on the surface of these substrates with an acid inhibitor will most likely not occur, making the sequence of pre-treatment important to the overall success. To ensure all carbon has been removed from the castings/heat-treated and/or hardened substrates, I recommend reverse current or anodic electro-cleaning after the hydrochloric acid pickle. The current flow and gassing at the anode will help pull the carbon away from the surface of the substrate prior to plating or finishing. Below is a typical pre-treatment sequence for iron castings, heat-treated and/or hardened substrates:

1. HOT ALKALINE SOAK CLEANER
Temperature - 150° to 180°F
Concentration - 8 to 12 oz/gal
Time - 4 to 6 minutes

2. CASCADING/COUNTER FLOW RINSING
Flow rate - 1 to 2 gallons per minute
Temperature - Ambient

3. HYDROCHLORIC ACID PICKLE
Temperature - Ambient
Concentration - 30 to 50% by volume
Time - 3 to 5 minutes
Pickle Pal - 2.0% by volume (Acid Inhibitor)

4. CASCADING/COUNTER FLOW RINSING
Flow rate - 1 to 2 gallons per minute
Temperature - Ambient

5. HOT ALKALINE ELECTRO-CLEANER
Temperature - 150° to 180°F
Concentration - 8 to 12 oz/gal
Time - 4 to 6 minutes
Current Density - 50 to 150 ASF

6. CASCADING/COUNTER FLOW RINSING
Flow rate - 1 to 2 gallons per minute
Temperature - Ambient

7. PLATE/FINISHING

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Processing High Carbon and Heat-treated Steel in an Alkaline non-Cyanide Zinc Process

Question:  I have two alkaline zinc baths, one is 1500 liters, zinc metal-8.9 g/l NaOH - 120 G/L and the other is of 2500 liters zinc metal-9.02 g/l NaOH- 130 G/L.  I am doing the same plating over plain carbon steel and alloy carbon steel. I am facing blisters when we heat the same component at 100° C . Delayed blistering is very common on these plated parts. The process sequence is:

(1) Hot soak (2) WR x 3 (3) Pickling (4) WRx2 (5) Hot Anodic (6) WRx3 (7) Acid activation (8) WRx29-NaOH neutralizer (10) Plating (11) Drag out (12) WRx313- Nitric dip (14) Tri-passivation (15) WRx2 (16) Sealer. 

Answer:  Some of the most difficult substrates to process through an alkaline non-cyanide zinc plating process are high carbon or heat-treated steels.  Although these substrates are challenging to process, improved adhesion is achievable with the proper pretreatment sequence.

There are two basic options for the pretreatment of high carbon or heat-treated steel substrates.  These options will perform exactly what you would expect from an excellent pretreatment system.  They will remove oils, scale and excessive smut/carbon that are found on high carbon or heat-treated substrates. 

Option #1 and Option #2 do have similarities.  First, both use an acid inhibitor in the hydrochloric acid pickle.  An acid inhibitor, specially formulated for use in electroplating lines, will greatly reduce or even eliminate the formation of carbon on the surface of the high carbon or heat-treated substrate.  Excessive carbon on the surface of the substrate will greatly decrease the overall adhesion of the zinc deposit.  Second, both options will cycle through an anodic cleaning station prior to entering into the alkaline non-cyanide plating solution.  Reverse current or anodic cleaning is critical for the removal of any carbon residue.  As mentioned previously, any carbon remaining on the substrate prior to plating will reduce adhesion of the zinc deposit.

OPTION #1

HOT ALKALINE SOAK CLEANER

Temperature - 65° to  85°C
Concentration - 60 to 90 g/L
Time - 4 to 6 minutes

             

HOT ALKALINE ELECTRO-CLEANER

Temperature - 65° to  85°C
Concentration - 60 to 90 g/L*
Time - 4 to 6 minutes
Current density - 2 to 15 amperes/dm2

                           

TWO TO THREE COLD WATER CASCADING OR COUNTER FLOWING RINSES

Flow rate - 4 to 8 Liters per minute
Temperature - Ambient

      

HYDROCHLORIC ACID PICKLE

Temperature - Ambient
Concentration - 30 to 50% by volume
Time - 3 to 5 minutes
Acid Inhibitor - 0.2% to 2.0% by volume

      

TWO TO THREE COLD WATER CASCADING OR COUNTER FLOWING RINSES

Flow rate - 4 to 8 Liters per minute
Temperature - Ambient

ELECTRO-CAUSTIC

Temperature - Ambient
Concentration - 100 to 150 g/L Sodium Hydroxide
Time - 1 to 2 minutes
Current density - 2 to 15 amperes/dm2

  

ALKALINE NON-CYANIDE PLATE

  

OPTION #2

HOT ALKALINE SOAK CLEANER

Temperature - 65° to  85°C
Concentration - 60 to 90 g/L
Time - 4 to 6 minutes

TWO TO THREE COLD WATER CASCADING OR COUNTER FLOWING RINSES

Flow rate - 4 to 8 Liters per minute
Temperature - Ambient

HYDROCHLORIC ACID PICKLE

Temperature - Ambient
Concentration - 30 to 50% by volume
Time - 3 to 5 minutes
Acid Inhibitor - 0.2% to 2.0% by volume

TWO TO THREE COLD WATER CASCADING OR COUNTER FLOWING RINSES

Flow rate - 4 to 8 Liters per minute
Temperature - Ambient

HOT ALKALINE ELECTRO-CLEANER

Temperature - 65° to  85°C
Concentration - 60 to 90 g/L*
Time - 4 to 6 minutes
Current density - 2 to 15 amperes/dm2

       

TWO TO THREE COLD WATER CASCADING OR COUNTER FLOWING RINSES

Flow rate - 4 to 8 Liters per minute
Temperature - Ambient

ALKALINE NON-CYANIDE PLATE

 

As you can see, Option #1 will most likely be the best sequence for your application.  A simple modification to the NaOH Neutralizer would be needed to improve the overall plating quality.

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Acid Chloride Zinc Post-Plate Staining

Question:  We acid zinc plate cast iron parts which are naturally covered with micro porosity holes. The parts are top coated with a thick film passivate and sealer. The problem is only during the summer months, after long storage and shipping, the parts exhibit a black spotting effect. This I believe is entrapment of plating solution which under extreme climate conditions - high humidity / temperature, migrates out and attacks the plating surface. We have been looking at the pickling process to understand the effects on the porosity. Are we over pickling? Or should we pickle longer to open the pores to enable better rinsing? We are looking at better ways to shot blast the components and investigating packaging. I am sure many platers have experienced this phenomenon - have you seen this and can you offer some thoughts? Is there a simple plating process adjustment I could try? We have just introduced additional spray rinsing where practical on the plating line.

Answer:  Unfortunately, this can be a common problem in the summer months when trying to process high porosity steel substrates. Salts from the pretreatment and plating processes can get entrapped in the pores of the substrate. Over time these salts will migrate through the zinc deposit, causing black discoloration or staining. Basically, due to the high temperature, humidity and salt remaining on or in the pores of the substrate, a corrosive environment is formed that discolors the zinc deposit.

Acid pickling high porosity steel can be difficult. Over pickling or etching high-porosity steel can cause a smut or contamination to form on the surface of the substrate. Under pickling will not remove all of the oxide scale deep within the pores and cause acid salts to become trapped. To improve the effectiveness of the acid pickle, use of an acid inhibitor along with an acid accelerating salt is recommended. Using these products together will allow for the hydrochloric acid pickle to aggressively remove the oxide scale but not allow for the substrate to be acid etched. These products can usually be offered from your chemical supplier. Rinsing after acid pickling is also important for consistent work. Maintaining a rinse water flow rate of 1 to 2 gallons per minute, along with air agitation, is highly recommended.

In regards to the plating process, I suggest maintaining your proprietary CARRIER or WETTING package on the high side of the operating range. A higher concentration of CARRIER or WETTER will improve the rinsability of the acid zinc chloride solution from the finished work.

Rinsing after plating is also a very important step for maintaining consistent work. Maintain 1 to 2 gallons per minute flow rate with air agitation to ensure no chloride solution remains on the finished work.

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Alkaline Non-cyanide Poor Cathode Efficiency

Question:  I have two alkaline zinc plating bath of capacity 1200Lts with Zn metal 8g/L, NaOH 120g/L and sodium carbonate 100g/L. With this I used to get 8-12microns thickness within 30 -35 min ( 5V 180 to 200Amps) but in the last 10 days it is taking 70-80 min to get 8-12 microns in both the baths with parameters being same as earlier. I checked the rectifier output; it is normal. I analyzed the solution concentration found as mentioned above. What might be causing this problem?

Answer:  Plating speed or cathode efficiency can be effected by a number of different variables within the alkaline non-cyanide plating solution. Please review the list of variables below:

 1. Zinc metal - Low concentrations of zinc metal will cause slow plating speed or poor cathode efficiency. Zinc metal operating parameters can vary between chemical supplier. Maintaining your zinc metal concentration at 12 to 15 g/L will help to improve plating speed, but it is recommended checking with your supplier if any proprietary additions will be needed after the increase in zinc metal.

 2. Temperature - Low bath temperatures can also cause slow plating speed or poor cathode efficiency. Maintaining a operating temperature of 26° to 35°C can help to improve plating speed.

 3. Sodium carbonates - High concentration of sodium carbonates will cause slow plating speed or poor cathode efficiency. Concentrations of sodium carbonates above 75 g/L can very quickly reduce plating speed. It is recommended maintaining your sodium carbonate levels below 75 g/L. A very common treatment for high sodium carbonates would be to “batch freeze” when weather is permits. If the weather does not permit, a bath cuts would be the your second best option.

 4. Proprietary additives – Over use of BRIGHTENERS and PURIFIERS can reduce overall plating speed or cathode efficiency. It is recommended having your supplier analyzing your plating solution for optimum additive concentrations.

Your bath analysis does indicate a low concentration of zinc metal and a high concentration of sodium carbonates. Making adjustments to the concentrations of zinc metal and sodium carbonates would be a great starting point for improving your overall plating speed.

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Staining Problems in Acid Zinc: Low Cloud Point

Question:  Why is a low cloud point causing staining problems in my acid zinc barrel?  What treatment is recommended and how can I prevent this problem in the future?

Answer:  Low cloud point is an indication of a high level of organic material (contamination) that has found its way into the plating solution.  Proprietary additives for acid zinc plating are typically formulated with surfactants and/or wetting agents that have high cloud point properties, which prevent the additives from “oiling out”.  When the cloud point falls below a given standard, (somewhere between 120° to 150°F), there is an indication of organic contamination which can interfere with the proprietary additives.  As your plating solution’s temperature approaches the cloud point, organic contamination becomes insoluble in the plating solution.  This insoluble material can coat the surface of the zinc deposit or even be co-deposited with the zinc, causing a white stain or a cloudy deposit.

A good way to improve/raise cloud point is to treat the plating solution with potassium permanganate.  A slurry of potassium permanganate and water is poured evenly over the top of the plating solution, using two pounds potassium permanganate per 1,000 gallons of plating solution.  The plating solution should be allowed to mix for at least one hour and filtered before plating is resumed.  Be sure to wear goggles, gloves and other protective clothing when handling potassium permanganate.  It will likely be necessary to add small amounts of proprietary additives back to the bath for optimum brightness. 

While permanganate treatments are effective at improving/raising cloud point, it is important to eliminate the source of contamination.  The most common culprit are overworked or spent cleaning solutions which cause oils and other organic contamination to be dragged down the line into the plating tank.   Increasing pretreatment rinse water flow rates can help, but dumping and making up new cleaners and then maintaining an appropriate dump/makeup schedule is the most effective way of preventing cloud point and staining problems.

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Rack Marks on Tubes in Alkaline Zinc

Question: I manufacture and finish conduit tubes for the electric industry.  The conduit is roughly 10 feet long and will have various diameters depending on the customer requirements.  We use alkaline non-cyanide zinc electrolyte for optimum plate distribution and thickness over the entire 10 foot piece.  Recently we have run into a plating issue on the conduit area where the rack hook meets each individual piece.  We are seeing a very dull/dark mark with no zinc thickness, it looks as though the piece has been burnt by the electrical contact point.  Reducing the current only makes the dull/dark mark larger.  Increasing the current does show improvement, but we are afraid we will burn or over-plate the work.  Any thoughts on what can be done to improve the plating quality.

Answer:  The situation you describe is actually a fairly common problem that can occur in high output alkaline non-cyanide zinc plating lines.  The problem, commonly called “rack marks”, is most likely caused by poor throwing power.   The area where the rack hook meets the conduit tube is typically a very low current density area.  Rack marks will worsen with reduced current and improve when current is increased. 

As always, the first step when troubleshooting a plating problem is to ensure that the part is being sufficiently cleaned prior to plate and to verify that plating bath chemistry (level of zinc and caustic soda in this case) is within the supplier’s specifications.  Levels of zinc and caustic soda affect both plating speed and throwing power.  Assuming that these check out okay, the next step is to examine the addition rates of the proprietary additives.

The most common cause of rack marks is low proprietary brightener additives. Generally, proprietary additives are added to the zinc plating solution based on amp-hours.  These additives control appearance/brightness, ductility and plate distribution of the zinc deposit.   However, in high drag-in/drag-out operations like plating tubes, it is often necessary to increase the addition rate of the additive(s) responsible for covering/throwing power.  Basically, these additives slow the zinc deposition rate in the high current density areas and increase it in the low current density areas – like where the rack meets the tube.    Increasing the addition rate of these additives will eliminate the dark mark and increase deposit thickness at the rack/tube interface, without increasing unwanted build-up of zinc on other areas of the tube.

Contact your supplier for their recommendation.  Often times, simply an increase in the main “brightener” component is all that is needed.  However in some cases, a separate additive developed specifically to improve throwing power is provided. 

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Dull Alkaline Zinc Deposits: Organic Contamination

Question:  I am an alkaline non-cyanide job shop plater in Michigan.  We are having a plating appearance issue that does not respond to any proprietary additives.  The problem is an overall lack of brightness in the deposit.  All of the work coming out of the line just does not have the snap that we and our customers are accustomed to seeing.  Our chemical supplier has analyzed our plating solution and has indicated that all proprietary additives are within the recommended operating ranges, but that the bath is contaminated with organics.  Their recommendation has been to treat the plating solution with carbon or potassium permanganate.  These treatments are effective but require extensive maintenance on the equipment that can slow down my production.  Are there any other treatments or additives available to help with organic contamination?

Answer:  Alkaline non-cyanide zinc plating solutions that do not respond to additions of proprietary additives usually suffer from one of two things.  They either contain excessive amounts of proprietary brighteners or have organic contamination (dragged in oils and soils from the pretreatment cleaning cycle).  Since an analysis of the plating solution did not show a high concentration of proprietary brighteners, let’s assume that the problem is caused by organic contamination.

Although treatments with potassium permanganate and carbon are extremely effective, they can be harsh on the maintenance crew.  Both are messy propositions with alkaline plating solutions, clogging up filters and taking away from production time.  A great alternative is treating the bath with commercial grade sodium hypochlorite.  Sodium hypochlorite is a strong oxidizing agent and is commonly found in or known as bleach.  Treatments with sodium hypochlorite are very effective on organic contamination and do not require heavy maintenance on the filtration system or long shut-down periods.

A full treatment is considered to be 10 gallons commercial grade sodium hypochlorite (12% active) per 1,000 gallons of plating solution.  Slowly add the sodium hypochlorite over the entire surface of the plating solution.  Good solution movement is recommended to ensure adequate oxidization of the organic contaminant.  Note that sodium hypochlorite is a strong oxidizing chemical and necessary safety precautions must be followed, such as wearing appropriate eye protection, gloves and other personal protection equipment.  A minimum of one hour shut-down time is necessary for this treatment. 

A “hypo” treatment along with small additions of your proprietary additives should bring back the brightness and luster that you expect from your alkaline non-cyanide zinc bath.

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The Zinc Plating Experts

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