Preliminary Requirements

Safety Requirements

WARNING

REFER ALSO TO THE SAFETY PRECAUTION IN THE SPM TASK 70-33-92-100-501.

IT IS THE RESPONSIBILITY OF THE OPERATOR TO OBTAIN AND OBSERVE THE MANUFACTURER'S MATERIAL SAFETY DATA SHEETS FOR CONSUMABLE MATERIALS. THESE CONTAIN INFORMATION SUCH AS, HAZARDOUS INGREDIENTS, PHYSICAL/CHEMICAL CHARACTERISTICS, FIRE, EXPLOSION, REACTIVITY, HEALTH HAZARD DATA, PRECAUTIONS FOR SAFE HANDLING, USE AND CONTROL MEASURES AND ALSO TO TAKE LOCAL REGULATIONS IN TO CONSIDERATION.

WARNING

THIS PROCEDURE INCLUDES THE USE OF SODIUM CYANIDE OR POTASSIUM CYANIDE. CYANIDE SALTS AND/OR SOLUTIONS ARE VERY POISONOUS AND WORK VERY QUICKLY. CYANIDE SALTS RELEASE HYDROCYANIC GAS WHEN MIXED WITH ACID. HYDROCYANIC GAS CAN KILL VERY QUICKLY.

Procedure

1. SUBTASK 70-33-92-160-001 Analytical Test Methods Used in the Control of Both Types of Nickel Plating Solution

   1. Estimation of Total Nickel Content - Volumetric Method with CoMat 01-090 ETHYL. DIAMINE TETRA ACETICACID .

      1. Pipette 10 ml of cooled sample into a 250 ml standard flask.

      2. Dilute to the mark with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and shake to mix fully.

      3. Pipette 50 ml of this solution into a suitable beaker and dilute to approximately 100 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

      4. Add 10 ml of CoMat 01-086 AMMONIUM HYDROXIDE SOLN NH4OH (SG 0.88) solution and 0.5 g of CoMat 01-089 MUREXIDE INDICATOR. Agitate the solution to mix.

      5. Titrate with N/5 solution of CoMat 01-090 ETHYL. DIAMINE TETRA ACETICACID until the light brown color changes through red to the deepest purple. Agitate the solution continuously while you do the titration.

         1. g/l total nickel = ml N/5 EDTA x 2.95.

   2. Estimation of Total Nickel Content - Gravimetric Method with Dimethyl Glyoxime.

      1. Pipette 10 ml of cooled sample into a 250 ml standard flask.

      2. Dilute to the mark with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and shake to mix fully.

      3. Pipette 25 ml of this solution into a suitable beaker and add a few CoMat 01-069 PRIMARY CLEANER. Agitate to dissolve the CoMat 01-069 PRIMARY CLEANER.

      4. Dilute to approximately 150 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

      5. Increase the temperature of the solution to 158 to 176 deg F (70 to 80 deg C). Add a small amount of 50 percent CoMat 01-086 AMMONIUM HYDROXIDE SOLN NH4OH to make the solution slightly alkaline.

      6. Add 20 ml of 1 percent CoMat 01-088 DI-METHYL GLYOXIME. Stir continuously while you add the CoMat 01-088 DI-METHYL GLYOXIME.

      7. Put the beaker in a warm place for 30 minutes to let the precipitate sink to the bottom of the beaker.

      8. Determine the nickel content by one of these methods:

         1. As weight of nickel oxide ash.

            1. Filter the solution through a 15 cm CoMat 02-012 FILTER PAPER and wash fully with hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

            2. Put the filter paper and filtrate (precipitate) into a clean, dry, weighed, crucible. Ignite at 1472+/- 45 deg F (800 +/- 25 deg C).

            3. When cool, weigh the crucible again and determine the weight of the nickel oxide ash.

            4. g/l total nickel = weight of ash x 786.

         2. As weight of dimethyl glyoxime complex.

            1. Filter the solution through a weighed gooch or sintered glass crucible (Porosity 3) dried at 212 to 230 deg F (100 to 110 deg C).

            2. Weight the crucible and contents. The dimethyl glyoxime complex contains 20.31 percent nickel.

            3. g/l total nickel = weight of precipitate x 203.

   3. Estimation of Boric Acid.

      1. Pipette 10 ml of cooled sample into a 250 ml standard flask.

      2. Dilute to the mark with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and shake to mix fully.

      3. Pipette 25 ml of this solution into a suitable beaker.

      4. Add 25 ml of boric acid additive mixture. For make-up, refer to the SPM TASK 70-33-92-100-501, SUBTASK 70-33-92-180-004.

      5. Agitate the solution to mix.

      6. Titrate with standard N/10 solution of CoMat 01-008 SODIUM HYDROXIDE NaOH (CAUSTIC SODA), SOLID until the color changes from pale green to deep pink.

      7. 1 ml of N/10 sodium hydroxide = 0.00618 g of boric acid. Therefore, g/l boric acid = ml N/10 sodium hydroxide x 6.18.

2. SUBTASK 70-33-92-160-002 Control of Watts-Type Nickel Plating Solution

   1. Estimate the Total Nickel by one of the methods in Step.

   2. Estimation of Nickel Chloride.

      1. Pipette 5 ml of cooled sample into a beaker and dilute to approximately 25 ml with demineralized water.

      2. NOTE

         To identify this end point needs care and practice because the green color of the solution and the white silver chloride precipitate mask the end point.

         Add a few drops of CoMat 01-092 INDICATOR and titrate carefully with N/20 solution of CoMat 01-059 SILVER NITRATE AgNO3 until the first red-brown silver chromate precipitate appears.

         Therefore, g/l nickel chloride = ml N/20 silver nitrate x 1.20.

   3. Calculation of Nickel Sulfate.

      1. To calculate the nickel sulfate concentration, subtract the amount of nickel combined as nickel chloride from the total nickel. To convert this answer to nickel sulfate, do these steps:

         1. Multiply the nickel chloride by 0.247 to give g/l nickel combined as chloride.

            1. That is, g/l nickel chloride x 0.247 = g/l nickel combined as chloride.

         2. Subtract combined nickel from total nickel (estimated by gravimetric analysis), and multiply the remainder by 4.78.

            1. That is, (g/l total nickel - g/l combined nickel) x 4.78 = g/l nickel sulfate.

   4. Estimation of Total Sulfate.

      1. Pipette 5 ml of cooled sample into a beaker.

      2. Dilute to approximately 150 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

      3. Add 10 ml of CoMat 01-006 HYDROCHLORIC ACID and agitate to mix.

      4. Boil the mixture for between 5 and 10 minutes.

      5. Slowly and carefully add 15 ml of CoMat 01-056 BARIUM CHLORIDE BaCl2x 2H2O. Stir continuously while you add the CoMat 01-056 BARIUM CHLORIDE BaCl2x 2H2O.

      6. Put the solution in a warm place for two hours to let the precipitate sink to the bottom of the beaker. Alternatively, let the precipitate form overnight at 59 to 77 deg F (15 to 25 deg C).

      7. Filter the solution through a 15 cm CoMat 02-011 FILTER PAPER and wash fully with hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER until the filtrate is free from chlorides.

      8. Put the filter paper and filtrate into a clean, dry, weighed crucible. Ignite at 1472 deg F (800 deg C).

      9. When cool, weigh the crucible again and determine the weight of the barium sulfate ash.

         1. Weight of ash in g x 0.411 = g sulfate. Therefore, g/l total sulfate = weight of ash x 82.2.

   5. Calculation of Sodium Sulfate.

      1. To calculate the sodium sulfate concentration, subtract the amount of nickel combined as nickel sulfate from the total sulfate. To convert the answer to sodium sulfate, do these steps:

         1. Multiply the nickel sulfate by 0.342 to give g/l sulfate combined as nickel sulfate. That is, g/l nickel sulfate x 0.342 = g/l combined sulfate.

         2. Subtract combined sulfate from total sulfate and multiply the remainder by 1.48 to give the sulfate content. That is, (g/l total sulfate - g/l combined sulfate) x 1.48 = g/l sodium sulfate.

   6. Estimate Boric Acid by the method in Step.

3. SUBTASK 70-33-92-160-003 Control of Sulfamate Type Nickel Plating Solution

   1. Estimate the Total Nickel by one of the methods in Step.

   2. Estimation of Nickel Chloride.

      1. Pipette 10 ml of cooled sample into a beaker and dilute to approximately 25 ml with demineralized water.

      2. NOTE

         To identify this end point needs care and practice because the green color of the solution and the white silver chloride precipitate mask the end point.

         Add a few drops of CoMat 01-092 INDICATOR and titrate carefully with N/20 solution of CoMat 01-059 SILVER NITRATE AgNO3 until the first red-brown silver chromate precipitate appears.

         1. g/l chloride (as chloride) = ml N/20 silver nitrate x 0.18.

         2. g/l nickel chloride = ml N/20 silver nitrate x 0.60.

   3. Calculation of Nickel Sulfamate.

   4. 1. To calculate the nickel sulfamate concentration, subtract the amount of nickel combined as nickel chloride from the total nickel. To convert this answer to nickel sulfamate, do these steps:

         1. Multiply the nickel chloride by 0.247 to give g/l nickel combined as chloride. That is, g/l nickel chloride x 0.247 = g/l nickel combined as chloride.

         2. Subtract combined nickel from total nickel (estimated by gravimetric analysis), and multiply the remainder by 5.5. That is, (g/l total nickel - g/l combined nickel) x 5.5 = g/l nickel sulfate.

   5. Estimate the Boric Acid by the method in Step.

4. SUBTASK 70-33-92-160-004 Control of Copper Plating Solution

   1. The control limits for the solution are:

      Free potassium cyanide 25 to 30 g/l.

      Metallic copper 35 to 45 g/l.

      pH 9.5 minimum.

   2. During plating, the pH of the solution can reduce to 9.5. If the pH reduces, add a small quantity of CoMat 01-130 POTASSIUM HYDROXIDE to increase the pH.

   3. To keep the free potassium cyanide at the specified amount, regularly add CoMat 01-107 POTASSIUM CYANIDE KCN95% MIN.

   4. The copper content is usually kept as specified by the dissolution of the copper anode. If the copper content is low, add CoMat 01-283 COPPER PLATING SOLUTION as necessary to increase the content to the specified level.

   5. To estimate the copper content:

      1. Transfer with a safety pipette, 5 ml of sample into a suitable beaker and, in a fume cupboard, carefully add 10 ml of CoMat 01-058 NITRIC ACID HNO3 and 10 ml of CoMat 01-043 SULFURIC ACID H2SO4.

      2. Boil until the mixture fumes.

      3. Cool and dilute to approximately 100 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

      4. Add 2 crystals of CoMat 01-287 UREA H2NCO.NH2.

         NOTE

         If copper is present in the mixture, the newly immersed part of the electrode will begin to plate with copper.

      5. Electrolyze at 1.5 amps for 30 to 45 minutes, on to a clean, weighed platinum electrode. At the end of this period, examine for absence of copper in the solution. Put more of the electrode into the mixture and continue the electrolysis for a short time.

      6. Wash the cathode in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and then in CoMat 01-007 ETHYL ALCOHOL C2H5OH (DENATURED). Dry the electrode and weigh again.

         Weight of copper x 200 = g/l metallic copper.

   6. To estimate the free cyanide content:

      1. Transfer with a safety pipette, 5 ml of sample into a suitable beaker and dilute to approximately 30 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

      2. Add 1 ml of CoMat 01-086 AMMONIUM HYDROXIDE SOLN NH4OH and a crystal of CoMat 01-097 POTASSIUM IODIDE KI.

      3. Titrate with N/10 silver nitrate (prepared from CoMat 01-059 SILVER NITRATE AgNO3) to a faint yellow cloudy appearance.

         1. 1 ml of N/10 silver nitrate = 0.013 g of potassium cyanide.

         2. Therefore, ml of silver nitrate x 0.013 x 200 = g/l of potassium cyanide. That is, ml of silver nitrate x 2.6 = g/l of potassium cyanide.