Preliminary Requirements

Safety Requirements

WARNING

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

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CARE MUST BE TAKEN WHEN YOU ADD COMPOUNDS THAT CONTAIN SOLID SODIUM HYDROXIDE TO WATER BECAUSE HEAT IS GIVEN OUT WHEN THE COMPOUND DISSOLVES. STRONGLY AGITATE (MAKE MUCH MOVEMENT OF) THE SOLUTION WITH AIR OR MECHANICAL METHODS AS YOU ADD THE COMPOUND TO THE SOLUTION. DO NOT ADD LARGE QUANTITIES OF THE COMPOUND TO ONE SMALL AREA OF THE TANK BECAUSE THE SOLUTION WILL BOIL.

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CHROMIC ACID IS STRONGLY OXIDIZING AND ENTAILS SOME FIRE RISK IN THE POSSIBLE SPONTANEOUS COMBUSTION OF ORGANIC MATERIALS, SUCH AS RAGS AND SAWDUST THAT HAVE ABSORBED CHROMIC ACID SOLUTION. SUCH CONTAMINATED MATERIALS SHOULD BE IMMERSED IN A SOLUTION OF SODIUM BISULPHIDE TO NEUTRALIZE THE CHROMIC ACID. THE SOLUTION SHOULD THEN BE DISPOSED OF AS SPECIAL WASTE, AND THE SOLID MATERIAL SHOULD THEN BE RINSED WITH WATER BEFORE DISPOSAL.

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AMMONIA, NITRIC ACID AND PERCHLORIC ACID MUST NOT BE FUMED TOGETHER IN THE SAME HOOD.

Procedure

1. SUBTASK 70-11-47-110-001 Concentrations of Reagents

   1. Concentration of acids and alkalis.

      1. When acids and alkalis are specified by name or chemical formula only, it must be understood that reagents of the specific gravities or concentration that follow are intended.

         1. CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE has a specific gravity of 1.18.

         2. CoMat 01-357 HYDROFLUORIC ACID (HF) has a concentration of 48 percent.

         3. CoMat 01-327 NITRIC ACID has a specific gravity of 1.42.

         4. CoMat 01-320 SULFURIC ACID has a specific gravity of 1.84.

         5. CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED has a specific gravity of 0.90.

      2. Desired specific gravities or concentrations of all other concentrated acids or alkalis will be stated whenever they are needed.

   2. Diluted acid and CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED, except when standardized, will be specified as a ratio, stating number of volumes of concentrated acid to be diluted with given number of volumes of water, as in the example that follows.

      Hydrochloric acid (5-95) means 5 volumes of concentrated CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE (specific gravity 1.18) diluted with 95 volumes of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

   3. Non-standardized solutions.

      1. Concentrations of non-standardized solutions prepared by dissolving given weight of solid reagent in solvent will be specified in grams of reagent/volume of solution, and that it must be understood that CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER is the solvent unless otherwise specified. For example, KMnO4 (100 g/l) means 100 g of KMnO4 salt dissolved in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER to a volume of one liter.

      2. NOTE

         In testing solutions reference to water must be understood to mean CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

         In case of certain reagents, concentration may be specified as a percentage weight, for example, H2O2 (30 percent) means a solution containing 30 g of H2O2 for every 100 g of solution. Other non-standardized solutions may be specified by name only and concentrations of such solutions will be governed by instructions for their preparation.

2. SUBTASK 70-11-47-180-001 Make-up Solutions in Standard Use

   1. Indicators.

      1. Alpha-Naptholbenzein.

         1. Dissolve 10 g of CoMat 01-407 INDICATOR in 100 ml of CoMat 01-410 ISOPROPYL ALCOHOL, REAGENT GRADE.

      2. Bromcresol green.

         1. Dissolve 0.10 g of CoMat 01-356 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED).

      3. Bromcresol purple.

         1. Dissolve 0.40 g of CoMat 01-310 INDICATOR in 50 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured).

      4. Bromphenol blue.

         1. Dissolve 0.10 g of CoMat 01-406 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured). (A commercially prepared indicator is available.).

      5. Bromthymol blue.

         1. Dissolve 0.10 g of CoMat 01-352 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured). (A commercially prepared indicator is available.).

      6. Diphenylamine.

         1. Dissolve 1.00 g of CoMat 01-405 INDICATOR in 100 ml of CoMat 01-320 SULFURIC ACID.

      7. Methyl orange.

         1. Dissolve 0.10 g of CoMat 01-037 INDICATOR in 100 ml of hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool and filter if necessary.

      8. Methyl purple.

         1. Dissolve 0.10 g of CoMat 01-404 INDICATOR in 100 ml of hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool and filter, if necessary.

      9. Methyl red.

         1. Dissolve 0.10 g of CoMat 01-064 INDICATOR in 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Filter if necessary.

      10. Ortho-Phenathroline-Ferrous sulphate.

          1. CoMat 01-403 INDICATOR is available commercially ready to use.

      11. Phenolphthalein.

          1. Dissolve 1,00 g of CoMat 01-011 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured).

      12. Sulfo-Orange.

          1. CoMat 01-402 INDICATOR is available commercially ready to use.

      13. Thymol blue.

          1. Dissolve 0.10 g of CoMat 01-401 INDICATOR in 20 ml of hot CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured). Dilute to 100 ml with CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured).

      14. Thymolphthalein.

          1. Dissolve 0.10 g CoMat 01-400 INDICATOR in 100 ml of 4-1 CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured).

      15. Titan yellow.

          1. Dissolve 0.50 g of CoMat 01-399 INDICATOR in 200 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 50 ml of CoMat 01-314 SODIUM HYDROXIDE (NaOH), REAGENT GRADE (SOLID) (15 percent) and dilute to 500 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER distilled or deionized water.

      16. Bromcresol green - Methyl red.

          1. Dissolve 0.1 g of CoMat 01-356 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) ethyl alcohol (denatured).

          2. Prepare methyl red as above.

          3. Mix 5 parts of Bromcresol Green (refer to (a)) with 1 part Methyl Red (refer to Step (9)(a)).

   2. Standardized solutions (Assay of chemical must be considered in weight of salt used for standard solutions). When the given make-up for a standard solution becomes impractical or inconvenient, such solution may be made in any convenient multiple or sub-multiple.

      1. Sodium Hydroxide and Potassium Hydroxide Solutions.

         1. Primary Standardization (standardization against potassium acid phthalate).

            1. Weigh three samples of CoMat 01-323 POTASSIUM ACID PHTHALATE which has been dried at 210 to 220 deg F (99 to 104 deg C) for 90 to 120 minutes and which has an assay of 99.95 percent or better, according to the formula that follows:

               Weight of potassium acid phthalate in grams = 8.5 x normality of hydroxide desired. Transfer each potassium acid phthalate sample to a clean 250 ml Erlenmeyer flask or 400 ml beaker.

            2. For each flask or beaker, do the subsequent procedure:

               1. Add 125 to 200 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dissolve the potassium acid phthalate salt.

               2. Add 2 to 3 drops of phenolphthalein indicator solution (Step A (11)) and titrate with hydroxide solution to a faint pink end-point that you can see continuously for 30 seconds minimum. Record titer.

            3. Calculations:

               N = (W x P)/(20.42 x V)

               Where:

               N = Normality of sodium hydroxide (NaOH) or potassium hydroxide (KOH).

               W = Weight of potassium acid phthalate.

               P = Percent purity of the potassium acid phthalate.

               V = Volume of hydroxide used.

            4. Average the three values obtained.

         2. NOTE

            Standardize the standard hydroxide solutions against potassium acid phthalate at least once every three months. These solutions may be used in an alternate method for standardization of acid solutions.

            Secondary Standardization (standardization against standardized acid solution).

            1. Pipette three 25 ml (or measure accurately by burette three 40 ml samples of standardized acid of similar normality to base into clean 250 ml Erlenmeyer flasks.

            2. For each flask, do the subsequent procedure:

               1. Add 75 ml water and 2 to 3 drops phenolphthalein indicator.

               2. Titrate with hydroxide solution to faint pink end-point that you can see continuously for 30 seconds minimum. Record titer.

            3. Calculations:

               N1 = (N2 x V2)/V1

               Where:

               N1 = Normality of hydroxide solution.

               N2 = Normality of standardized acid.

               V1 = Average volume of hydroxide solution used in the three titrations

               V2 = Volume of standardized acid sample.

            4. Average the three values obtained.

      2. Acid solutions.

         1. Primary standardization:

            Weigh out accurately in to 400 ml beakers, three samples of CoMat 01-237 TRIS (HYDROXY METHYL)AMINO METHANE according to the formula that follows:

            Weight of tris (hydroxy methyl) amino methane in grams = 5 x normality of acid desired.

            Dissolve each sample in 200 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

            Add 5 to 6 drops of bromcresol green-methyl red and titrate to first appearance of faint rose color.

            Calculations:

            N = Normality of acid.

            W = Weight of tris (hydroxy methyl) amino methane.

            P = Percent purity of tris (hydroxy methyl) amino methane.

            V = Volume of acid used.

            N = WP/12.114V.

            Average the three values obtained.

         2. NOTE

            Use previously standardized base solution.

            NOTE

            Standardize the standard acid solutions against tris (hydroxy methyl) amino methane at least once every three months. These solutions may be used as an alternate method for standardization of base solutions.

            Secondary standardization:

            Pipette three 25 ml (or measure accurately by burette three 40 ml) samples of the acid into clean 250 ml Erlenmeyer flasks.

            Add 75 ml of water and 2 or 3 drops of phenolphthalein indicator.

            Titrate with standard base solution of approximately similar normality to faint pink end point which persists for at least 30 seconds. Record titer.

            Calculations:

            N1 = Normality of acid.

            N2 = Normality of standardized base solution.

            V1 = Volume of acid used.

            V2 = Average volume of the standard base solution used in three titrations.

            N1 = V2N2/V1.

      3. Potassium permanganate solution.

         1. NOTE

            The make-up of a 1-19 sulfuric acid solution is 1 volume of CoMat 01-320 SULFURIC ACID diluted with 19 volumes of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

            Standardization.

            Weigh three samples of CoMat 01-398 SODIUM OXALATE dried at 210 to 220 deg F (99 to 104 deg C) for 90 to 120 minutes and having an assay of 99.95 percent or better according to the formula that follows:

            Weight of sodium oxalate in grams = normality of potassium permanganate.

            Dissolve in 250 ml of a 1-19 sulfuric acid solution.

            Run a preliminary titration on one sample by heating to 130 to 140 deg F (54 to 60 deg C) and titrating to a permanent faint pink end point with potassium permanganate solution.

            To the remaining solution of sodium oxalate, add from a burette about 95 percent of the potassium permanganate solution used in the paragraph above. Heat to 130 to 140 deg F (54 to 60 deg C) and continue titration to permanent faint pink end point. Record titer.

            Calculations.

            N = Normality of potassium permanganate.

            V = Average volume of potassium permanganate (second and third titrations only).

            P = Purity of sodium oxalate.

            W = Weight of sodium oxalate.

            N = WP/6.700V.

      4. Sodium thiosulfate solutions.

         1. Primary standard potassium dichromate 0.1N.

            Weigh accurately 4.9040 g of CoMat 01-384 POTASSIUM DICHROMATE dried at 300 to 350 deg F (149 to 177 deg C) for 60 to 90 minutes.

            Dissolve in 200 to 300 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, transfer to flask, and dilute to 1 l.

         2. NOTE

            A starch solution can be purchased ready to use or make a paste of 1.0 g of CoMat 01-385 STARCH and a small quantity of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 150 ml of hot water and boil for 2 to 3 minutes.

            Standardization:

            Pipette three 25 ml (or measure accurately by burette three 40 ml) samples of primary potassium dichromate solution into 500 ml glass-stoppered flasks.

            Add 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, 2 to 3 g of CoMat 01-308 POTASSIUM IODIDE (KI) and 10 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE hydrochloric acid.

            Put the stopper in the flask, mix to dissolve iodide, and let it stand in a closed cabinet for 8 to 10 minutes.

            Remove the stopper and add 150 to 200 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, rinsing the sides of the flask.

            Titrate with sodium thiosulfate, mix constantly until reddish brown changes to yellow green.

            Add 4 to 6 ml of starch solution and continue titrating until the color changes sharply from blue to light green. Add thiosulfate dropwise as end point nears.

            Record titers and average.

            Calculations.

            N = Normality of sodium thiosulfate.

            V = Volume of sodium thiosulfate.

            W = Normality of potassium dichromate.

            P = Volume of potassium dichromate.

            N = WP/V.

      5. Silver nitrate solutions.

         1. Standardization.

            Weigh three 0.1 g samples of CoMat 01-319 SODIUM CHLORIDE which has been dried at 203 to 239 deg F (95 to 115 deg C) for two hours and which has an assay of 99.8 percent or better.

            Dissolve in 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER distilled or deionized water.

            Add 2 to 3 drops of 10 percent CoMat 01-321 POTASSIUM CHROMATE (CHLORIDEFREE) solution.

            Titrate with silver nitrate solution until the first permanent reddish tint appears.

            Record titer.

            Calculations.

            M = Molarity of silver nitrate solution.

            W = Weight of sodium chloride.

            P = Purity of sodium chloride.

            V = Volume of silver nitrate.

            M = WP/5.845V.

            Average the three values obtained.

      6. Standardization of 0.1M EDTA.

         1. NOTE

            The make-up of a 1-1 hydrochloric acid solution is 1 volume of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE hydrochloric acid diluted with 1 volume of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER distilled or deionized water.

            Weigh accurately 3.269 g of CoMat 01-351 ZINC METAL into a 1000 ml volumetric flask. Add 50 ml of a 1-1 hydrochloric acid solution to dissolve the zinc and dilute to the mark with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Mix well. Save for future EDTA standardization.

         2. Pipette a 25 ml aliquot of standard CoMat 01-351 ZINC METAL (0.05M) into a 250 ml beaker. Add concentrated CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED, drop by drop, until a white precipitate appears and remains for a few seconds. Then add 5 ml of CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED ammonium hydroxide in excess and 50 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER distilled or deionized water. Add a pinch of CoMat 01-109 INDICATOR. Titrate with EDTA solution to a purple end point.

            Calculations.

            M = Molarity of EDTA solution.

            V = Volume of EDTA (ml) used in titration.

            M = 1.25/V.

3. SUBTASK 70-11-47-180-002 Accuracy of Volumetric Measurement

   1. When instructions read DILUTE TO XX VOLUME, it must be understood that a volumetric flask of xx volume must be used to measure that volume.

   2. Volume measurements must be maintained in accordance with values listed below, unless otherwise specified. When pipettes and burettes or volumetric flasks are specified, or when procedure indicates use of such equipment by means of descriptive terms such as TITRATE, no tolerances in measurement will be permitted outside of those inherent in measuring devices.

      1. Measurement tolerances.

         1. For volumes less than 25 ml, the tolerance permitted is plus or minus 20 percent.

         2. For volumes 25 to 100 ml, the tolerance permitted is plus or minus 10 percent.

         3. For volumes 101 to 500 ml, the tolerance permitted is plus or minus 5 percent.

         4. For volumes over 500 ml, the tolerance permitted is plus or minus 2 percent.

   3. When dissolving samples in acids, larger additions of acids, other acids or CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER than specified may be used if difficulty arises in dissolving chips.

4. SUBTASK 70-11-47-180-003 Procedure and Accuracy of Weighing

   1. The analytical balance must have a sensitivity of 1/10 mg.

   2. All weights of original samples which are specified by procedure must be weighed to plus or minus 0.0005 g. Weights of all other samples must be weighed to plus or minus 0.0002 g.

   3. Accuracy of all other weighing measurements must be held within plus or minus 0.5 of unity in last digit stipulated.

      1. Examples.

         1. Desired grams is 223. Permissible range is 222.5 to 223.5.

         2. Desired grams is 22.7. Permissible range is 22.65 to 22.75.

         3. Desired grams is 600. Permissible range is 599.5 to 600.5.

   4. It is important to keep pans, beams, bearings and all parts of case clean and free from dust and chemicals.

   5. Weight values of original specimens specified in procedure is approximate.

      1. Example:

         Desired grams 0.5000. Permissible range is 0.4500 to 0.5500.

   6. Before you start to weigh, be sure that the balance is properly adjusted. If necessary, turn the leveling screws at the base of the case until the spirit level on the back of the pillar shows balance is level. Note whether knife-edges are in correct positions with respect to bearings, and whether the pointer rests at zero point on the scale. Check the chain to be sure that it is tight around the drum or in column.

   7. Stop the lower beam by slowly turning the knurled knob at the bottom of the case in a counterclockwise direction. Make sure that the pointer is still at zero point when the pans are resting on pan rests. Make adjustments if necessary.

   8. With the balance case closed, release the pan rests. The pointer must come to rest two divisions to the left of center. If it does not, increase or decrease the weight of the right hand pan by the chain adjusting knob hanging from the circular vernier. Then correct the zero setting by adjusting the screw on the upper right side of the balance case.

   9. Place a sample to be weighed on the left hand pan and increase the weights on the right hand pan, the rider on notched beam, and the vernier until the needle again rests at two divisions to the left of center.

5. SUBTASK 70-11-47-180-004 Precautions for Use of the Balance

   1. The balance must rest on a firm support which is free from mechanical vibration.

   2. Direct sunlight must not fall on the balance as it will cause irregularities and errors in weighing.

   3. All weights must be made in order, with weights tried one after another in their correct order.

   4. Final adjustments and all observations must be made with the balance case closed to prevent errors occurring from air currents. When the balance is not used, the case must always be closed.

   5. Substances to be analyzed must never be placed directly on the balance pan but on a watch glass or aluminum pan.

   6. Care must be taken not to load the balance more than its capacity.

   7. Hot or cold objects must not be weighed until they have come to room temperature or to the temperature of the air in the balance case. Air currents from a hot body made it weigh too little, while condensation or moisture on a cold body make it look like it is too heavy.

6. SUBTASK 70-11-47-180-005 Recording of Results

   1. All calculations, measurements and results of analyses, and tests of all kinds must be initially recorded in log books or computer media.

   2. When data is necessary for the calculations of results of analyses, this data must be recorded in a work log book. For example, when a chemical procedure calls for a titration to be done, it must be understood to mean that initial and final titration readings will be recorded. Logbook specimen weight entries must be recorded to four decimal places unless otherwise specified. Weight can be recorded to one or two places if the places that follow are zeros.

      1. 0.0500 can be recorded as 0.05.

      2. 0.5000 can be recorded as 0.5.

      3. 0.2500 can be recorded as 0.25.

7. SUBTASK 70-11-47-180-006 Primary Standards

   1. Analysis of solutions has been predicated on use of chemicals of known purity meeting these standards. Chemicals of equivalent standards will give equivalent results. If chemicals of known lower standards are used, there may have to be an equivalent adjustment in calculations. A special danger is that contamination in chemicals of lower standards can introduce errors in results.

   2. The salts given below must be Reagent grade or ACS approved grade.

      1. CoMat 01-323 POTASSIUM ACID PHTHALATE.

      2. CoMat 01-384 POTASSIUM DICHROMATE.

      3. CoMat 01-237 TRIS (HYDROXY METHYL)AMINO METHANE.

      4. CoMat 01-133 SILVER NITRATE CRYSTALS.

      5. CoMat 01-398 SODIUM OXALATE.

      6. Iron of known purity.

      7. Alloy standards.

8. SUBTASK 70-11-47-180-007 Platinum Ware

   1. Precautions.

      1. Never use platinum ware in contact with mixtures of hydrochloric and nitric acids, acid ferric chloride, easily reducible metals, alkali hydroxides, sulfides, compounds of lead, tin, bismuth, arsenic, antimony, zinc or mixtures which release chlorine.

      2. Prevent heating platinum in contact with carbon and compounds of phosphorus.

      3. Prevent heating over 1950 deg F (1066 deg C) for long amounts of time.

      4. Prevent bending platinum or squeezing to remove melts.

      5. Never use knifes, files, or glass rods to remove melts.

   2. Cleaning.

      1. Electrodes.

         1. NOTE

            The make-up of a 1-1 nitric acid solution is 1 volume of CoMat 01-025 NITRIC ACID HNO3, TECHNICAL GRADE nitric acid diluted with 1 volume of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER distilled or deionized water.

            Put fully in a 1-1 nitric acid solution.

         2. NOTE

            The make-up of a 1-1 ethyl alcohol (denatured) solution is 1 volume of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) diluted with 1 volume of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

            Flush in a 1-1 ethyl alcohol (denatured) solution.

         3. Flush with water.

         4. Dip in CoMat 01-239 ETHYL-ALCOHOL (DENATURED).

         5. Drain and ignite remaining alcohol on the electrode.

         6. Heat the electrode to a dull red in the oxidizing flame of gas burner.

         7. For nickel plate, boil the electrode in CoMat 01-025 NITRIC ACID HNO3, TECHNICAL GRADE before you do Step (a).

         8. Make straight with a wooden form if necessary.

      2. Crucibles and Dishes.

         1. Place 1 or 2 scoops of CoMat 01-397 POTASSIUM PYROSULFATE or CoMat 01-182 NICKEL STRIP SALT in the crucible or dish and fuse gently over an oxidizing flame.

         2. Pour out the molten flux.

         3. NOTE

            The make-up of a 1-1 hydrochloric acid solution is 1 volume of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE diluted with 1 volume of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

            Wash in boiling CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER or in boiling 1-1 hydrochloric acid solution.

         4. Polish dull surfaces with 75 to 100 grit sea-sand made moist with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and applied with fingers or a soft cloth.

         5. Put the crucibles and dishes back into shape with wooden or plastic forms.

9. SUBTASK 70-11-47-180-008 Use of Polyethylene, Polypropylene and Teflon Ware

   1. Polyethylene and polypropylene are generally interchangeable. These materials must be used wherever high concentrations of CoMat 01-357 HYDROFLUORIC ACID (HF) are present. They must not be used where hot oxidizing acids (such as CoMat 01-327 NITRIC ACID) are involved. Polyethylene may be safely used at temperatures up to 175 deg F (79 deg C) and polypropylene up to 275 deg F (135 deg C). Beakers can be used over a steam bath, in a sand bath or heated by electrical jackets.

   2. Teflon ware is also resistant to CoMat 01-357 HYDROFLUORIC ACID (HF) but has the added feature of resisting hot oxidizing acids. Also, Teflon can be safely heated to 600 deg F (316 deg C) and is better for use where large volumes of solutions must be evaporated. Teflon beakers can be heated by all methods for polyethylene or polypropylene, and can also be set on wire gauze in contact with medium temperature hot plates.

10. SUBTASK 70-11-47-180-009 Sampling of Solutions

    1. General.

       1. New solutions must be sampled and tested, and results reported before use, unless otherwise specified. Solutions already in use must be sampled, tested and the results calculated on a regular schedule.

       2. Approved persons must do the sampling after they check Analysis and Addition Cards to find if additions have been made before.

       3. Solutions not in use for a length of time longer than usual periods for testing, are not necessary for testing until they are used again.

    2. Sampling procedures.

       1. Solutions must be adjusted to full tank level as shown by the marker and when mixed, by mechanical means or by hand, a sample must be taken. Acid solutions which are lower than the full level can be sampled and adjusted to the full level at the time of additions.

       2. A sufficiently long 0.5000in. (12.70 mm) diameter open tube, which is chemically inactive to the solution, must be flushed in the solution to be tested. The tube in a vertical position must then be put fully into the solution in several locations, closed at the upper end and removed. Each time the solution in the tube must be moved to a container which has been flushed in the solution and which can be sealed and identified.

       3. Molten salt baths or other processes which can not be adapted to the above sampling procedure can be sampled by ladling with heat resistant containers or other suitable means.

       4. All unwanted conditions monitored in the tank or its solution must be noted. Corrective action must be taken.

11. SUBTASK 70-11-47-180-010 Additions to Solutions

    1. The chemist must make out an Analysis and Addition Card for each sample. The Analysis and Addition Card must show analysis, necessary additions for best concentration, tank identification and date of sampling.

    2. The Analysis and Addition Card must be placed on or near the tank as soon after sampling as possible at which time the card before must be removed and put in a permanent file.

    3. Analysis and Addition Cards must give space to make the entries that follow.

       1. Additions.

       2. Quantity of each addition.

       3. Date and hour of each addition.

       4. Initials of person who makes to addition.

12. SUBTASK 70-11-47-180-011 Plating Solutions Index, Refer to SUBTASK 70-11-47-180-035

    1. This index lists in numerical order, those cleaning and plating solutions that must be tested. The name of each solution is also included.

    2. NOTE

       Depending on the amount of use each solution gets, the frequency can be increased or decreased based on experience. In any event, samples must be analyzed often enough to be sure that there is adequate control.

       The critical property or concentration of each solution that must be controlled is given along with the suggested frequency with which each must be checked.

    3. NOTE

       Solutions which are not in this list do not require regular analysis and filling to keep correct concentration. Most of these solutions will be discarded and replaced when dirty or no longer effective.

       The test procedure used is listed in the last column.

13. SUBTASK 70-11-47-170-012 Test Method Index

    1. Below is the index of solution test method numbers (refer to Step) and their SUBTASK numbers.

       1. Test Method P-1 is given in Step.

       2. Test Method P-4 is given in Step.

       3. Test Method P-6 is given in Step.

       4. Test Method P-8 is given in Step.

       5. Test Method P-9 is given in Step.

       6. Test Method P-14 is given in Step.

       7. Test Method P-17 is given in Step.

       8. Test Method P-18 is given in Step.

       9. Test Method P-22 is given in Step.

       10. Test Method P-30 is given in Step.

       11. Test Method P-33 is given in Step.

       12. Test Method P-36 is given in Step.

       13. Test Method P-55 is given in Step.

       14. Test Method P-59 is given in Step.

       15. Test Method P-60 is given in Step.

       16. Test Method P-66 is given in Step.

       17. Test Method P-79 is given in Step.

       18. Test Method P-82 is given in Step.

       19. Test Method P-90 is given in Step.

       20. Test Method P-91 is given in Step.

       21. Test Method P-100 is given in Step.

14. SUBTASK 70-11-47-180-013 Test Method P-1, Acid Solutions

    1. Apparatus.

       1. Autotitrator or manual titration.

    2. Solutions.

       1. Sodium hydroxide (1.ON).

          1. Dissolve 40.0 g of CoMat 01-314 SODIUM HYDROXIDE (NaOH), REAGENT GRADE (SOLID) in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Dilute to 1000 ml with water.

          2. Standardize the solution. Refer to Step, Step 5.B.(1).

       2. Indicator.

          1. Dissolve 1.0 g of CoMat 01-011 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED).

    3. Procedure.

       1. Pipette a sample into a 250 ml flask as follows.

          1. 10.00 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE.

          2. 5.00 ml of CoMat 01-327 NITRIC ACID.

          3. 5.00 ml of CoMat 01-320 SULFURIC ACID.

          4. 2.00 ml of CoMat 01-364 PHOSPHORIC ACID or CoMat 01-466 PHOSPHORIC ACID.

       2. Add 75 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 2 to 3 drops of indicator solution.

       3. Titrate with sodium hydroxide solution (1.ON) to a permanent faint pink color.

       4. NOTE

          Adjustment of volume and estimation of factor is permitted in order to get a suitable titer.

          Record titer.

    4. Calculations.

       In these calculations abreviations are use as follows:

       HCl means hydrochloric acid.

       NaOH means sodium hydroxide.

       H2SO4 means sulfuric acid.

       HNO3 means nitric acid.

       H3PO4 means phosphoric acid.

       SG means specific gravity.

       deg Be means degrees Baume.

    5. 1. Percentage of HCl (SG 1.16) by volume = ml NaOH x N x 0.980.

          Percentage of HCl (20 deg Be) by volume = ml NaOH x N x 0.980.

       2. Percentage of H2SO4 (SG 1.84) by volume = ml NaOH x N x 0.560.

       3. Percentage of HNO3 (SG 1.41) by volume = ml NaOH x N x 1.268.

          Percentage of HNO3 (42 deg Be) by volume = ml NaOH x N x 1.268.

       4. Percentage of H3PO4 (SG 1.58) by volume = ml NaOH x N x 2.070.

       5. NOTE

          Acid quality can cause factors to vary.

          To determine the factor of the acid actually being used in the solution:

          Percentage of H3PO4 (SG 1.69) by volume = ml NaOH x N x 0.3439.

          1. Take samples of the undiluted acid and by use of the volumes list in Paragraph C.(1), titrate with 1.0 N NaOH as in Paraagraphs C.(2) and (3).

          2. Do three analyses for each acid.

          3. The factors for 5 ml of acid will be different than those for 10 ml or more; therefore, a factor should be determined for each different volume of the same acid.

             Calculation of Acid Factor = 100 percent/NAOH titer x NaOH Normality.

15. SUBTASK 70-11-47-180-014 Test Method P-4, Carbonates in Cyanide Plating Solutions

    1. Solutions.

       1. Barium chloride (10 percent).

          1. Dissolve 100 g of CoMat 01-394 BARIUM CHLORIDE (BaCl2) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       2. Hydrochloric acid (0.5N).

          1. Add 43.0 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 500 ml of water. Cool and dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Standardize the solution. Refer to Step, Step 5.B.(2).

    2. Procedure.

       1. Pipette a 10.0 ml specimen into a 250 ml beaker, dilute with 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, and heat to 110 to 140 deg F (43 to 60 deg C).

       2. Add barium chloride solution (10 percent) refer to Step A.(1)(a), as you stir, until no more precipitate forms.

       3. Allow the precipitate to settle, filter the solution, and add a few drops of barium chloride solution (10 percent) to the first portion of the filtrate to determine whether the precipitation is complete.

       4. Wash with hot distilled or deionized water and transfer the filter paper and precipitate to the beaker in which the precipitation was originally made.

       5. Add 50 ml of hot distilled or deionized water and a few drops of methyl orange indicator. Refer to Step, Step A.(7)(a).

       6. Add 1/2 - 1 tablet of CoMat 02-189 COMPRESSED PAPER.

       7. Titrate with hydrochloric acid (HCl) (0.5N) to a permanent pink. Refer to Step A.(2).

       8. Record titer.

    3. Calculations.

       Na2CO3 is sodium carbonate.

       K2CO3 is potassiun carbonate.

       1. Oz/gal Na2CO3 = ml HCl x N of HCl x 0.706.

       2. Oz/gal K2CO3 = ml HCl x N of HCl x 0.923.

16. SUBTASK 70-11-47-180-015 Test Method P-6, Alkali Cleaning Solution

    1. Apparatus.

       1. pH meter.

       2. Magnetic stirrer and bar.

       3. Volumetric flasks, 1000 ml, 500 ml.

       4. Burette 50 ml.

       5. Beakers 250 ml.

    2. Solutions.

       1. Sulfuric acid (1.ON).

          1. Add 28.0 ml of CoMat 01-320 SULFURIC ACID to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool and dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Standardize the solution. Refer to Step, Step 5.B.(2).

       2. Hydrochloric acid (0.5N).

          1. Add 43.0 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool and dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Standardize the solution. Refer to Step, Step 5.B.(2).

       3. Hydrochloric acid (0.1N).

          1. Add 8.5 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, and dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER .

          2. Standardize the solution. Refer to Step, Step 5.B.(2).

       4. Phenolphthalein indicator solution, refer to Step, Step 5.A.(11).

       5. Bromcresol green - Methyl red indicator solution, refer to Step, Step 5.A.(16).

       6. Hydrochloric acid (0.01N).

          1. Add 1.7 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER in a 2000 ml volumetric flask. Dilute to volume.

          2. Standardize the solution. Refer to Step Step 5.B.(2)(b).

    3. Make up of cleaner factor.

       1. For dry or solid cleaners.

          1. Weigh three parts of cleaner which represent the low, medium and high concentrations as usually used and calculated to make 500 ml of each of the concentrations necessary.

             Weight of test specimen (g) = 3.75 x conc of cleaner (oz/gal).

          2. Put the salts in plastic volumetric flasks, each containing 300 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Heat to 195 to 205 deg F (91 to 96 deg C) to dissolve the salts. Cool at room temperature and dilute to 500 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Mix well.

          3. NOTE

             This test specimen is used in Step C.(1)(d) and Step D.(1) that follows:

             Pipette a 10 ml test specimen of the lowest concentration and add phenolphthalein indicator solution and titrate with CoMat 01-320 SULFURIC ACID solution (1.ON) to a colorless endpoint and monitor the titer. Adjust the test specimen size or acid normality, as necessary, to give a titer of 10 ml minimum.

          4. Pipette three test specimens of each concentration, size as given in Step (c), and add 25 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 2 to 8 drops of phenolphthalein indicator solution and titrate to the colorless end point, refer to Step, Step 5.A.(11). Record titers.

             Calculate the factors for each test specimen as follows:

             a = concentration of cleaner necessary in oz/gal.

             b = ml standard acid.

             c = normality of standard acid.

             Factor = a/bc.

             Average the nine results. This is the factor to be used in Step E.(1).

       2. For cleaners supplied as liquids.

          1. Measure three parts of cleaner which represents the low, medium and high concentrations as usually used and calculated to make 1000 ml of each of the concentrations necessary.

          2. The volume of the test specimen ml equals ten times the concentration of the cleaner in percent. For example, 9 percent = 90 ml/liter.

          3. Add the above parts to 1000 ml plastic volumetric flasks which contain 200 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool to room temperature, if necessary, and mix well. Fill to 1000 ml with water and mix well.

          4. Pipette a 10 ml test specimen of the lowest concentration (for CoMat 01-300 ALKALI CLEANER (GENERAL PURPOSE), use a 50 ml specimen). Do as in Step C.(1)(c), to find the test specimen size to use in Steps C.(2)(e) and D.(1). For CoMat 01-300 ALKALI CLEANER (GENERAL PURPOSE) specimens, use 0.1N hydrochloric acid solution and bromcresol green - methyl red indicator solution.

          5. Pipette three test specimens of each concentration and add 25 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 2 to 8 drops of phenolphthalein indicator solution and titrate to the colorless end point. For concentrations of 2.5 percent or less, use a pH meter to find the end point of 8.2. Record titers. For CoMat 01-300 ALKALI CLEANER (GENERAL PURPOSE) specimens, add 5 to 10 drops of bromcresol green - methyl red indicator solution and titrate with O.1N hydrochloric acid solutions to a straw orange end point. Record titer.

          6. a = concentration of cleaner necessary in percent.

             b = ml standard acid.

             c = normality of standard acid.

             Factor = a/bc.

          7. Average the 9 results. This is the factor to be used in Step E.(2).

    4. Procedure to give the concentration.

       1. Pipette the test specimen as given in Step C.(1)(c) or C.(2)(d) into a 250 ml Erlenmeyer flask. Add 25 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 2 to 8 drops of phenolphthalein indicator solution.

       2. Titrate with the correct standard acid to the colorless end point, or as applicable. For concentrations of 2.5 percent or less, use a pH meter to find the end point of 8.2. Record titer.

    5. Calculations.

       1. Concentration of dry cleaner.

          a = ml acid.

          b = normality of acid.

          F = factor of cleaner.

          oz/gal = abF.

       2. Concentration of liquid cleaner.

          a = ml acid.

          b = normality of acid.

          F = factor of cleaner.

          percent volume = abF.

    6. Specimen size for regular analysis.

       1. Dry alkalis.

          1. Use a 10 ml specimen size for the dry alkalis that follow:

             CoMat 01-022 SODIUM HYDROXIDE NaOH (SOLID).

             CoMat 01-129 POTASSIUM HYDROXIDE KOH.

             CoMat 01-130 POTASSIUM HYDROXIDE.

             CoMat 01-138 ALKALI CLEANER (HEAVYDUTY).

             CoMat 01-139 ALKALI CLEANER (HEAVYDUTY).

             CoMat 01-141 ALKALI DRAWING COMPOUNDREMOVER.

             CoMat 01-176 ALKALI CLEANER (MEDIUMDUTY).

             CoMat 01-218 ALKALI CLEANER.

             CoMat 01-302 ALKALI CLEANER PHOSPHATE-FREE.

             CoMat 01-303 ALKALI CLEANER PHOSPHATE-FREE(HEAVY DUTY).

             CoMat 01-304 ALKALI CLEANER (LIGHTDUTY).

             CoMat 03-107 POTASSIUM HYDROXIDE.

          2. Use a 20 ml specimen size for the dry alkali that follows:

             CoMat 01-217 ALKALI CLEANER (LIGHTDUTY).

       2. Liquid alkalis.

          1. Use a 5 ml specimen size for CoMat 01-008 SODIUM HYDROXIDE NaOH (CAUSTIC SODA), SOLID.

          2. Use a 20 ml specimen size for CoMat 01-301 ALKALI CLEANER (GENERALPURPOSE).

          3. Use a 25 ml specimen size for CoMat 01-299 SYNTHETIC CLEANER.

          4. Use a 50 ml specimen size for CoMat 01-300 ALKALI CLEANER (GENERAL PURPOSE).

17. SUBTASK 70-11-47-180-016 Test Method P-8, Copper Plating Solution (Cyanide Type)

    1. Apparatus.

       Electrolysis apparatus.

    2. Solutions.

       1. Silver nitrate (0.1N).

          1. Dissolve 16.9890 g of CoMat 01-133 SILVER NITRATE CRYSTALS, previously dried for 1 to 2 hours at 205 to 215 deg F (96 to 102 deg C), in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml. Store in a dark container.

       2. Potassium iodide (10 percent).

          1. Dissolve 100 g of CoMat 01-308 POTASSIUM IODIDE (KI) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       3. Ceric sulfate (0.1N).

          1. Add 28 ml of CoMat 01-320 SULFURIC ACID slowly to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER in a large beaker. Add 53 g of CoMat 01-425 CERIC SULFATE and stir until dissolved. Dilute to 1000 ml with distilled or deionized water, mix thoroughly, and transfer to a glass-stoppered bottle. It may be standardized at once.

          2. Standardization.

             1. Standardize against freshly standardized 0.1N ferrous ammonium sulfate. Refer to Step 4. Pipette 25 ml ferrous ammonium sulfate solution into a 500 ml flask that contains 100 ml cold sulfuric acid (1-4). Add 1 to 2 drops of CoMat 01-403 INDICATOR, O-phenanthroline indicator and titrate with ceric sulfate solution (refer to Step (3)) until the color changes from reddish to colorless or greenish.

                Normality Ceric sulfate =

                (N Ferrous ammonium sulfate x 25)/ml ceric sulfate

       4. Ferrous ammonium sulfate (0.1N). Add 30 ml of CoMat 01-320 SULFURIC ACID (H2SO4) slowly to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 39.5 g of CoMat 01-423 FERROUS AMMONIUM SULFATE Fe(NH4)2(SO4)2, stir until dissolved, and dilute to 1000 ml with distilled or deionized water. Filter before the standardization.

          1. Standardization.

             1. Standardize against standard 0.1N potassium dichromate (refer to Step 5.). Pipette 25 ml ferrous ammonium sulfate solution into a 500 ml flask that contains 100 ml of sulfuric acid H2SO4 (1-4). Add 10 ml CoMat 01-364 PHOSPHORIC ACID H3PO4 (85 percent) and 1 to 2 drops of diphenylamine indicator. Refer to Step (7). Titrate to a purple end point with standard 0.1N potassium dichromate solution (refer to Step (5)).

                Normality Ferrous ammonium sulfate =

                (ml potassium dichromate x 0.1)/25

       5. Standard potassium dichromate.

          1. Dry 5g pure CoMat 01-384 POTASSIUM DICHROMATE K2Cr207 at 225 to 230 deg F (107 to 110 deg C) for no less than two hours. Weigh 4.9035g of dried salt, transfer to 600 ml beaker, dissolve in 400 ml warm CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml.

       6. CoMat 01-403 INDICATOR. Purchase ready to use.

       7. Diphenylamine indicator.

          1. Dissolve 1.00 g of CoMat 01-405 INDICATOR (C6H5)2NH in 100 ml of CoMat 01-320 SULFURIC ACID H2SO4.

       8. EDTA (0.1M) Comat CoMat 01-350 ETHYLENE DIAMINETETRA-ACETIC ACID (EDTA). Purchase ready to use. Store in a plastic container.

       9. Buffer solution (pH10).

          1. Dissolve 70 g of CoMat 01-424 AMMONIUM CHLORIDE NH4C1 in 570 ml CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED NH40H. Dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Store in a plastic container.

       10. Murexide indicator CoMat 02-190 CHEMICAL TABLETS. Purchase in tablet form.

    3. Procedure.

       1. Metallic Copper.

          1. Pipette a 10 ml specimen into a 300 ml beaker.

          2. Under a hood, add 10 ml of CoMat 01-320 SULFURIC ACID and 15 ml of CoMat 01-327 NITRIC ACID HNO3. Cover with a raised cover glass.

          3. Heat to heavy sulfurous fumes. If the solution turns dark, add 2 ml of nitric acid and again take to sulfurous fumes. Again add small amount of nitric acid until the color of the solution remains bluish-green when it gives off sulfurous fumes.

          4. Cool, wash cover glass and sides of beaker with distilled or deionized water, and add 150 ml of water. Add 10 to 15 ml of nitric acid.

          5. Plate at 3 to 5 amperes on weighed platinum electrodes until all the copper is removed from the solution. To determine if all the copper is plated out of the solution, raise the level of the solution with water and check for further deposition of copper on the cathode.

          6. With the current ON, remove cathode and rinse it thoroughly in distilled or deionized water. Rinse cathode in alcohol (1-1) and alcohol.

          7. 

             CAUTION

             DO NOT OXIDIZE THE PLATE.

             Ignite and burn off the alcohol.

          8. Weigh the cathode.

       2. Copper (EDTA) Alternate Method.

          1. Pipette a 2 ml specimen into a 250 ml flask.

          2. Under a hood, add 2 ml of nitric acid and 2 ml of sulfuric acid. Place on a hot plate and heat to dense white fumes. Cool.

          3. Slowly and carefully add 10 ml of distilled or deionized water. Cool.

          4. Add 8 ml of buffer solution and add the buffer solution dropwise until the solution has turned dark blue.

          5. Add 75 ml of distilled or deionized water. If the solution becomes slightly turbid, add more buffer solution dropwise.

          6. Add 1 tablet of CoMat 02-190 CHEMICAL TABLETS Murexide indicator. Shake to dissolve.

          7. Titrate with CoMat 01-350 ETHYLENE DIAMINETETRA-ACETIC ACID (EDTA) to a permanent blue-violet end point.

          8. Record the titer.

       3. Free Sodium Cyanide.

          1. Pipette a 100 ml specimen into a 250 ml flask.

          2. Add 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 5 ml of potassium iodide solution (10 percent). Refer to Step B.(2).

          3. Titrate with silver nitrate solution (0.1N) (refer to Step B.(1)) to a faint permanent turbidity.

          4. Record the titer.

       4. Rochelle Salt or Rocheltex.

          1. Pipette duplicate 1 ml specimens into 500 ml flasks. Add 75 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 25 ml of CoMat 01-320 SULFURIC ACID.

          2. Run duplicate blanks simultaneously with specimens:

             Add 25 ml of sulfuric acid to 75 ml of distilled or deionized water in 500 ml flasks, and follow the procedure in Steps (c) thru (g).

          3. Add glass beads and boil very gently until the residue dissolves (30 to 60 minutes). Maintain the solution in the flask at a constant level by washing down the sides with water from time to time. This also prevents the precipitate from clinging to the walls.

          4. Remove from hot plate and cool to room temperature. Add 1 to 2 drops of CoMat 01-403 INDICATOR and titrate with 0.1N ceric sulfate solution (refer to Step B.(3) until the color changes from orange or pale rose to colorless. Add ceric sulfate solution dropwise as only a few drops are necessary.

          5. 

             CAUTION

             THE SOLUTION SUPERHEATS.

             NOTE

             If while boiling, the solution changes from yellow to colorless, pipette an additional 25 ml of ceric sulfate solution into the flask.

             Pipette 25 ml of ceric sulfate solution into the flask and add water until the solution level is about 1 to 1 1/2in. from the bottom of the flask. Boil gently for 30 to 60 minutes.

          6. Remove from hot plate and cool to room temperature. Add CoMat 01-403 INDICATOR and titrate with 0.1N ferrous ammonium sulfate solution (refer to Step B.(4)) until the color changes from yellow thru colorless to the orange or pale rose end point.

          7. Record the titer.

       5. Hydroxide. Refer to Test Method P-9 in Step.

       6. Carbonate. Refer to Test Method P-4 in Step.

    4. Calculation.

       1. Oz/gal Metallic Cu = grams Cu x 13.4 Oz/gal CuCN =.

          grams Cu x 18.9 Oz/gal CuCN.

          where Cu means copper and CuCN means copper cyanide.

       2. Oz/gal Metallic copper = ml EDTA x 0.43.

       3. Oz/gal Free NaCN = ml 0.1N silver nitrate = 0.131.

       4. Oz/gal Rochelle salt = (a - b)/a x N x 131.0 x c/25.

          ml/gal Rocheltex = (a - b)/a x N x 5370.0 x c/25.

          Where:

          a = ml ferrous ammonium sulfate necessary to titrate blank.

          b = ml ferrous ammonium sulfate necessary to titrate specimen.

          c = ml ceric sulfate used in specimens.

          N = Normality of ceric sulfate.

18. SUBTASK 70-11-47-180-017 Test Method P-9, Hydroxides in Cyanide Solutions

    1. Solutions.

       1. Hydrochloric Acid (0.5N).

          1. Add 43.0 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE HCl to 500 ml of water and dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Mix well.

          2. Standardization - Acid solution refer to Step Step 5.B.(2).

       2. Lamotte Sulfo - Orange Indicator CoMat 02-211 INDICATOR. Purchase ready to use.

    2. Procedure.

       1. Pipette 10.0 ml test specimens into three 250 ml flasks. Number flasks 1, 2 and 3. Also label and pipette a 10.0 ml water blank and add 3 to 5 drops of hydrochloric acid solution (refer to Step A.(1)) to the blank.

       2. NOTE

          Unless the indicator volumes are equal, the color produced will not match.

          Add 10 ml of distilled or deionized water and 7 to 9 drops of LaMotte Sulfo-Orange indicator to each solution.

       3. To the first specimen, add standard hydrochloric acid solution (refer to Step A.(1)) from a burette until a definite yellow color similar to the blank is produced which does not change appreciably with additional hydrochloric acid solution. Record the original end point.

       4. Use this first specimen as a color standard and titrate specimens 2 and 3 until the color is produced.

       5. Record the titer.

    3. Calculations.

       1. Oz/gal NaOH = Average ml HCl x N of HCl x 0.535.

       2. Oz/gal KOH = Average ml HCl x N of HCl x 0.749.

19. SUBTASK 70-11-47-180-018 Test Method P-14, Silver Plating Solutions (Cyanide-type)

    1. Apparatus.

       Electrolysis equipment.

    2. NOTE

       In this test method, sodium thiocyanate solution may be written as NaSCN; silver nitrate solution as AgNO3 and hydrochloric acid solution as HCl.

       Solutions.

       1. Ferric ammonium sulfate.

          1. Soak 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER with CoMat 01-390 FERRIC AMMONIUM SULFATE. Add CoMat 01-327 NITRIC ACID (free of nitrous acid by heating) until the solution is clear and a pale yellow color.

       2. Sodium thiocyanate (0.1M).

          1. Dissolve 8.1 g of CoMat 01-391 SODIUM THIOCYANATE (NaSCN) in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml. Pipette 25 ml of silver nitrate solution (0.1M) into a 250 ml Erlenmeyer flask. Add 5 ml of CoMat 01-327 NITRIC ACID, 1 ml of ferric ammonium sulfate solution and 50 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Titrate with sodium thiocyanate solution until a permanent reddish brown tinge appears in the solution which is being shaken.

             Molarity of NaSCN = 25 x Molarity of AgNO3/ml NaSCN.

       3. Silver nitrate (0.1M).

          1. Dissolve in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER 17.0 g of CoMat 01-360 SILVER NITRATE (AgNO3) dried before for 1 to 2 hours at 205 to 215 deg F (96 to 102 deg C) and dilute to 1000 ml. Keep in a dark container.

          2. Standardize the solution. Refer to Step, Step 5.B.(5).

       4. Potassium iodide solution.

          1. Dissolve 100 g of CoMat 01-308 POTASSIUM IODIDE (KI) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 1.0 g of CoMat 01-322 POTASSIUM HYDROXIDE. Keep in a dark container.

       5. Hydrochloric acid (0.5N).

          1. Add 43.0 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml.

          2. Standardize the solution. Refer to Step, Step 5.B.(2).

       6. Barium chloride (10 percent).

          1. Dissolve 100 g of CoMat 01-394 BARIUM CHLORIDE (BaCl2) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER distilled or deionized water.

    3. Procedure.

       1. Metallic silver (Volumetric, alternate procedure).

          1. Pipette a 5 ml test specimen of clear solutions into a 250 ml flask.

          2. Under a hood, add 20 ml of CoMat 01-320 SULFURIC ACID and 15 ml of CoMat 01-327 NITRIC ACID.

          3. Shake the flask and boil until all white precipitate which forms has dissolved.

          4. Decrease the temperature and add 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER slowly and cautiously.

          5. Decrease the temperature to room temperature and add 1.0 ml of ferric ammonium sulfate solution and titrate with sodium thiocyanate (0.1M) solution.

          6. The first visual color change occurs about one percent before the equivalent point. After the first color change has occurred, continue titration carefully with much movement until a reddish brown tinge shows which is permanent when you shake the solution.

          7. Record titer.

       2. Metallic silver (electrolytic).

          1. NOTE

             For Solution Code 52, use a 100 ml specimen.

             Pipette a 5 ml test specimen of clear solution into a 300 ml electrolytic beaker.

          2. Add 150 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, 4 to 6 g of CoMat 01-322 POTASSIUM HYDROXIDE and 9 to 11 g of CoMat 01-392 POTASSIUM CYANIDE (KCN).

          3. Plate at 1.8 to 2.2 amps on weighed platinum electrodes until all silver is removed from the solution. To find out if all the silver has been plated out of the solution, increase the level of solution with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and check for more deposits of silver on the cathode.

          4. With the current on, remove the cathode and flush with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Clean the cathode in baths one after the other, of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, 1-1 alcohol and alcohol. Supply ignition and burn off the alcohol.

          5. Cool and weigh the cathode.

       3. Free potassium cyanide.

          1. Pipette a 5 ml sample into a 250 ml flask, add 100 ml of (CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 2 ml of potassium iodide solution (10 percent).

          2. Titrate with silver nitrate solution (0.1M) to a faint permanent turbidity against a dark background.

          3. Record titer.

       4. Potassium hydroxide.

          1. Pipette three 10 ml specimens into 250 ml flasks. Number the specimens 1, 2 and 3. Also label and pipette a 10 ml CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER blank and add 3 to 5 drops of hydrochloric acid solution (0.5N) to the blank.

          2. NOTE

             Unless the indicator volumes are equal, the color produced will not be the same.

             Add 10 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 7 to 9 drops of CoMat 01-402 INDICATOR to each flask.

          3. To the Number 1 specimen, add hydrochloric acid solution (0.5N) from a burette until a yellow color equivalent to the blank is produced which does not change much with additions of the hydrochloric acid solution. Record the titer of the first end point.

          4. Use flask number 1 as a color standard. Titrate the Number 2 and 3 specimens with hydrochloric acid solution (0.5N) until you get the same yellow color as in flask number 1.

          5. Record titers.

       5. Potassium carbonate.

          1. Pipette a 10 ml sample into a 250 ml beaker, dilute with 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and heat to 110 to 140 deg F (43 to 60 deg C).

          2. Add barium chloride solution (10 percent) while you mix until no more precipitate forms.

          3. Permit the precipitate to go to the bottom of the beaker. Filter the liquid through CoMat 02-210 FILTER PAPER and add a few drops of barium chloride solution (10 percent) to the first portion of filtrate to find if precipitation is complete.

          4. Clean with hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and move the filter paper and precipitate to the beaker in which precipitation was initially done.

          5. Add 50 ml of hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and a few drops of methyl orange indicator solution.

          6. Titrate with hydrochloric acid solution (0.5N) until you get a permanent pink color.

          7. Record titer.

    4. Calculations.

       1. Metallic silver (volumetric).

          1. Oz/gal metallic silver = (ml NaSCN)(Molarity of NaSCN)(2.88).

       2. Metallic silver (electrolytic).

          1. For Solution Code 52:

             Oz/gal metallic silver = (weight of silver)(1.33).

          2. For Solution Code 53:

             Oz/gal metallic silver = (weight of silver)(26.70).

       3. Free potassium cyanide.

          1. Oz/gal free KCN = (ml AgNO3)(Molarity of AgNO3)(3.48).

       4. Potassium hydroxide.

          1. Oz/gal KOH = (average HCl)(Normality of HCl)(0.749).

       5. Potassium carbonate.

          1. Oz/gal potassium carbonate = (ml HCl)(Normality of HCl)(0.923).

20. SUBTASK 70-11-47-180-019 Test Method P-17, Nickel Plate Solution

    1. Apparatus.

       pH meter.

    2. Solutions.

       1. Sodium cyanide (1.0M).

          1. Dissolve 49.0 g of CoMat 01-307 SODIUM CYANIDE (NaCN) in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml.

          2. Standardization.

             Pipette 10 ml of sodium cyanide solution into a 250 ml Erelenmeyer flask, add 50 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 10 to 15 drops of potassium iodide solution (10 percent).

             Titrate with silver nitrate solution (0.1M) to a faint permanent turbidity.

             Molarity of NaCN soln. = ml AgNO3 soln. x molarity of AgNO3 x 0.2.

       2. Silver nitrate (0.1M).

          1. Dissolve 16.9890 g of CoMat 01-360 SILVER NITRATE (AgNO3), dried for 1 to 2 hours at 205 to 215 deg F (96 to 102 deg C), in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml. Store in a dark bottle.

          2. Standardize silver nitrate solutions. Refer to Step, Step B.(5).

       3. Potassium iodide (10 percent).

          1. Dissolve 100 g of CoMat 01-308 POTASSIUM IODIDE (KI) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 1.0 g of CoMat 01-322 POTASSIUM HYDROXIDE. Store in a dark bottle.

       4. CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED.

       5. Ethylenediamine tetra-acetic acid, Sodium salt (EDTA) (0.1M).

          1. Weigh out 37.2 g of CoMat 01-350 ETHYLENE DIAMINETETRA-ACETIC ACID (EDTA) pure dihydrate salt and 6.0 g of CoMat 01-314 SODIUM HYDROXIDE (NaOH), REAGENT GRADE (SOLID). Dissolve in a final volume of 1 l of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Standardization of 0.1M ethylenediamine tetraacetic acid.

             Weigh accurately 3.269 g of CoMat 01-351 ZINC METAL into a 1000 ml volumetric flask. Add 50 ml of 1-1 hydrochloric acid solution to dissolve the zinc and dilute to mark with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Mix well. Save for future EDTA standardization.

             Pipette a 25 ml aliquot of standard zinc (0.05M) into a 250 ml beaker. Add concentrated CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED, drop by drop, until a white precipitate appears and stays for a few seconds. Then add 5 ml of CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED in excess of 50 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add a pinch of CoMat 01-109 INDICATOR. Titrate with EDTA solution to a purple end point.

             Molarity of EDTA = 1.25/ml of EDTA.

       6. Citric acid.

          1. Dissolve 200 g of CoMat 01-311 CITRIC ACID in a cooled mixture of 900 ml CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 100 ml of CoMat 01-043 SULFURIC ACID H2SO4.

       7. Murexide indicator. Purchased CoMat 02-190 CHEMICAL TABLETS (0.4 mg).

    3. Procedure.

       1. Nickel (Procedure A).

          1. Pipette 5.00 ml of plating solution into a 250 ml flask. Add 25 ml of citric acid, 50 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED dropwise until the solution just turns a clear blue.

          2. Add from a burette 2.00 ml of silver nitrate solution (0.1M). If the solution becomes turbid add CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED dropwise until the solution turns clear again. Add 10 to 15 drops of potassium iodide solution (10 percent).

          3. Titrate with sodium cyanide solution (1.0M) to clear amber. Add silver nitrate solution one ml at a time until the solution turns turbid again. Titrate dropwise with sodium cyanide solution (1.0M) until the solution turns clear again.

          4. NOTE

             For low nickel metal concentrations, use 50 ml specimens.

             Record total titer and molarity of both sodium cyanide and silver nitrate.

       2. Nickel (Procedure B).

          1. Pipette 5.00 ml of plating solution into a 250 ml flask.

          2. Add 50 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, 10 ml of citric acid solution and from a burette 15 ml of CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED .

          3. Add 1 CoMat 02-190 CHEMICAL TABLETS and mix to dissolve.

          4. Titrate with sodium cyanide solution (1.0M) to a purple pink end point.

          5. NOTE

             For low metal concentrations, use a 50 ml specimen.

             Record titer.

       3. Nickel (Alternative Non-cyanide for Solution Codes 30 and 55).

          1. Pipette a 2 ml sample into a 250 ml beaker, add 75 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and mix.

          2. Add 10 ml of CoMat 01-306 AMMONIUM HYDROXIDE (NH4OH),CONCENTRATED and two CoMat 02-190 CHEMICAL TABLETS.

          3. Titrate with EDTA solution (0.1M) until the solution color changes quickly to purple.

    4. Calculations.

       In these calculations, NaCN means sodium cyanide and AgNO3 means silver nitrate.

       1. Nickel metal (Procedure A).

          1. Oz/gal nickel metal =.

             ((NaCN titer x M of NaCN) - (AgNO3 titer x M of AgNO3)) x 0.392.

       2. Nickel metal (Procedure B).

          1. NOTE

             For low nickel concentration with a 50 ml sample, use a factor of 0.078.

             Oz/gal nickel metal = NaCN titer x M of NaCN x 0.392.

       3. Nickel metal (Electroless).

          1. Oz/gal nickel metal = NaCN titer x M of NaCN x 0.0.78.

       4. Nickel metal (Alternative non-cyanide procedure).

          1. Oz/gal nickel metal = ml EDTA x M of EDTA x 3.92.

21. SUBTASK 70-11-47-180-020 Test Method P-18, Free Cyanide in Process Solutions

    1. Solutions.

       1. Silver nitrate (0.1M).

          1. Dissolve 16.9890 g of CoMat 01-360 SILVER NITRATE (AgNO3) dried for 1 to 2 hours at 205 to 215 deg F (96 to 102 deg C), and dilute to 1000 ml. Keep in a dark container.

          2. Standardize, Silver nitrate solutions, refer to Step, Step 5.B.(5).

       2. Potassium iodide (10 percent). Dissolve 100 g of CoMat 01-308 POTASSIUM IODIDE (KI) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 1.0 g of CoMat 01-322 POTASSIUM HYDROXIDE. Keep in a dark container.

    2. Procedure.

       1. Free Sodium cyanide or Potassium cyanide.

          1. Pipette a 10 ml sample into a 250 ml flask. Add 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 5 ml of potassium iodide solution.

          2. NOTE

             For solutions with high concentration of cyanide use a 5 ml sample of solution to be tested.

             Titrate with standard silver nitrate solution to a faint permanent turbidity against a dark background.

    3. Calculations.

       1. Free sodium cyanide.

          1. 10 ml sample.

             In these calculations, NaCN means sodium cyanide, KCN means potassium cyanide and AgNO3 means silver nitrate.

             Oz/gal free NaCN = ml AgNO3 solution (0.1M) x 0.131.

          2. 5 ml sample.

             Oz/gal free NaCN = ml AgNO3 solution (0.1M) x 0.262.

       2. Free potassium cyanide.

          1. 10 ml sample.

             Oz/gal free KCN = ml AgNO3 solution (0.1M) x 0.174.

          2. 5 ml sample.

             Oz/gal free KCN = ml AgNO3 solution (0.1M) x 0.348.

22. SUBTASK 70-11-47-180-021 Test Method P-22, Chromium Plating Solution and Anodize Touch-Up Solution (CoMat 02-136 Chromate Conversion Salt or CoMat 03-125 Chromate Conversion Salt)

    1. Apparatus.

       Centrifuge and accessories.

    2. Solutions.

       1. Starch solution.

          1. Purchase ready to use or make a paste of 1.0 g CoMat 01-385 STARCH and a small quantity of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 150 ml of hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and boil for 2 to 3 minutes.

       2. Sodium thiosulfate (0.1N).

          1. Dissolve 25 g of CoMat 01-383 SODIUM THIOSULFATE in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 0.1 g of CoMat 01-382 SODIUM CARBONATE for each liter of solution and permit it to stand for one week before standardization.

          2. Standardize the solution. Refer to Step, Step 5.B.(4).

       3. Barium chloride (10 percent).

          1. Dissolve 100 g of CoMat 01-394 BARIUM CHLORIDE (BaCl2) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       4. Sulfate solution A.

          1. Special sulfate solution A purchased ready to use, or dilute 420 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       5. Sulfate solution B.

          1. Special sulfate solution B purchased ready to use, or dissolve 300 g of CoMat 01-395 BARIUM CHLORIDE - 2 HYDRATE in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       6. Potassium iodide solution (10 percent).

          1. Dissolve 100 g of CoMat 01-308 POTASSIUM IODIDE (KI) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 1.0 g of CoMat 01-322 POTASSIUM HYDROXIDE. Store in a dark bottle.

       7. Ammonium bifluoride solution (10 percent).

          1. Dissolve 100 g of CoMat 01-396 AMMONIUM BIFLUORIDE in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Store in a plastic container.

    3. Procedure.

       1. Chromic acid.

          1. Pipette a 10 ml test specimen into a 250 ml volumetric flask and dilute with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Pipette a 10 ml test specimen of this diluted solution into a 250 ml beaker or flask.

          3. Add 10 ml of ammonium bifluride solution, 50 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 25 ml of potassium iodide solution.

          4. Add 10 ml of CoMat 01-320 SULFURIC ACID (1-1) and titrate immediately with standard sodium thiosulfate solution to a light yellow green color.

          5. Add 1 to 2 ml of starch solution and continue titrating until the dark blue color changes quickly to clear green.

          6. Record titer.

       2. CoMat 02-136 CHROMATE CONVERSION SALT or CoMat 03-125 CHROMATE CONVERSION SALTS.

          1. Pipette 5.0 ml of solution into a 250 ml Erlenmeyer flask.

          2. Add 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, 25 ml of potassium iodide solution and 10 ml of CoMat 01-320 SULFURIC ACID (1-1). Mix.

          3. Titrate with standard sodium thiosulfate solution (0.1N) to a light lemon yellow color.

          4. Add 1 to 3 ml of starch solution.

          5. Continue the titration with standard sodium thiosulfate solution until the dark color changes quickly to a clear green.

       3. pH of solution. Refer to Test Procedure P-82, Step.

       4. Sulfates (a modification of the Kocour Procedure).

          1. Cool the sample to room temperature.

          2. Place the special glass centrifuge tube in the aluminum shield and add 5 ml of sulfate solution A to the tube.

          3. Pipette a 20 ml sample of solution to be tested into the tube.

          4. Stopper the tube and shake heavily for 1 minute. Replace the tube into the centrifuge shield with its adaptor and permit it to stand for 5 minutes.

          5. Balance the tubes in pairs and centrifuge at about 1000 rpm until all possible sediment has been collected in the bottom of the tube.

          6. Record the reading of the level in the tube. This reading is a blank.

          7. Add 5 ml of sulfate solution B to the sample.

          8. Stopper the tube and shake with much movement for 1 minute. Replace the tube in the shield and permit it to stand for 5 minutes.

          9. Balance the tubes again and centrifuge at about 1000 rpm until the level of precipitate in the tube remains constant with continued centrifuging.

          10. NOTE

              For solutions which have a concentration of sulfate resulting in readings off the scale, a smaller specimen can be used in Step (c), and the final reading, Step (j) minus Step (f) can be multiplied by 20 divided by the volume.

              Record the reading of the level. Subtract blank (f) for the corrected reading.

       5. Sulfates (Optional Procedure).

          1. Pipette a 5 ml sample into a 400 ml beaker and add 175 to 250 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Add 10 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE, 10 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) and 10 ml of CoMat 01-057 ACETIC ACID CH3COOH.

          3. Boil for 10 minutes and add 10 ml barium chloride solution. Boil for 2 to 3 minutes more, remove from the hot plate and let it stand for 2 to 3 hours.

          4. Filter on CoMat 02-011 FILTER PAPER, washing paper and precipitate well unit the filtrate is not acid.

          5. Move the paper and precipitate to a weighed porcelain crucible.

          6. Char and ignite at 1000 deg F (538 deg C) for 1 hour.

          7. Cool and weigh.

    4. Calculations.

       1. Oz/gal chromic acid (CrO3) = ab (11.1).

          where:

          a = ml of sodium thiosulfate.

          b = normality sodium thiosulfate.

       2. CoMat 02-136 CHROMATE CONVERSION SALT or CoMat 03-125 CHROMATE CONVERSION SALTS.

          1. Oz/gal chromate conversion salt = ab (1.62).

             where:

             a = ml of standard sodium thiosulfate.

             b = normality of sodium thiosulfate.

       3. Read the pH directly from the meter.

       4. Oz/gal sulfate, Kocour sulfate test procedure. Change the corrected reading to oz/gal. Each numbered division on the tubes represents 0.1 oz/gal of sulfate and each subdivision of it equals 0.02 oz/gal.

       5. Oz/gal sulfate, optional precipitate procedure = (a-b) (11.28).

          where:

          a = weight crucible and precipitate.

          b = weight crucible.

23. SUBTASK 70-11-47-180-022 Test Method P-30, Silver Strike Solution

    1. Apparatus.

       Electrolysis apparatus.

    2. Solutions.

       1. Silver nitrate (0.1N). Dissolve 16.9890 g of CoMat 01-360 SILVER NITRATE (AgNO3), dried before for 1 to 2 hours at 205 to 215 deg F (96 to 102 deg C), in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml. Store in a dark container.

       2. Potassium iodide (10 percent). Dissolve 100 g of CoMat 01-308 POTASSIUM IODIDE (KI) in 1000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1000 ml. Add 1,0 g of CoMat 01-322 POTASSIUM HYDROXIDE. Store in a dark bottle.

    3. Procedure.

       1. Metallic silver.

          1. Pipette 100 ml of solution into a 300 ml electrolytic beaker.

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

          3. Add 5 g of CoMat 01-322 POTASSIUM HYDROXIDE and 10 g of CoMat 01-392 POTASSIUM CYANIDE (KCN). Mix to dissolve.

          4. Plate at 1.8 to 2.2 amps on weighed platinum electrode until all silver is removed from the solution. To find out if all the silver is removed, increase the level of the solution with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and check for more deposition of silver on cathode.

          5. With current on, remove the cathode, flush fully with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Dip the cathode in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER distilled or deionized water; then dip in alcohol. Ignite and burn off the alcohol.

          6. Cool and weigh the cathode.

       2. Free potassium cyanide.

          1. Pipette a 5 ml sample into a 250 ml flask, add 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 2 ml of potassium iodide solution (10 percent).

          2. Titrate with silver nitrate solution (0.1N) to a faint permanent turbidity.

    4. Calculations.

       In these calculations KCN means potassium cyanide and AgNO3 means silver nitrate.

       1. Metallic silver.

          1. Oz/gal metallic silver = weight silver x 1.33.

       2. Free potassium cyanide.

          1. Oz/gal free KCN = ml AgNO3 (0.1N) x 0.348.

24. SUBTASK 70-11-47-180-023 Test Method P-33, Nitric Acid, Ammonium Bifluoride or Hydrofluoric Acid Solution

    1. Apparatus.

       1. Nalgene (polypropylene) pipettes.

       2. Nalgene beakers, 200 ml or 300 ml and 400 ml.

       3. Nalgene 100 ml or 1000 ml volumetric flasks.

       4. Magnetic stirrer and bars or discs or equivalent procedure giving satisfactory agitation.

       5. Calibrated thermometers 0 to 220 deg F (-18 to 104 deg C), stainless steel dial or plastic coated glass.

       6. Glass automatic or standard burette for ferrous sulfate solution.

       7. Nalgene automatic leveling or standard burettes for sodium hydroxide.

       8. Atomic Absorption Spectrophotometer (AA) for testing titanium content.

       9. Applicable hollow cathode or electroless discharge lamp for testing titanium content.

    2. Solutions.

       1. Primary standard Nitric acid solutions (approximately 3N, 200 ml/liter).

          1. To 2000 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, add slowly and cautiously 700 ml of concentrated CoMat 01-327 NITRIC ACID and dilute to 3500 ml; mix well. This can be measured in a large graduate as the solution must be standardlized against CoMat 01-237 TRIS (HYDROXY METHYL)AMINO METHANE.

          2. Standardization. Nitric acid solutions. (Refer to Step, Step 5.B.(2)).

       2. NOTE

          AR HF is an Analytical Reagent Grade hydrofluoric acid (48 to 51 percent).

          Optional synthetic standard Solution Code 50 (40 percent (that is, 400 ml/l) CoMat 01-327 NITRIC ACID), 2 percent (that is, 20 ml of CoMat 01-132 HYDROFLUORIC ACID HF /1 = 29 ml AR/l) CoMat 01-357 HYDROFLUORIC ACID (HF) by volume.

          1. To a 1000 ml Nalgene volumetric flask which contains approximately 300 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, add 400 ml of CoMat 01-327 NITRIC ACID and 29.6 ml of CoMat 01-357 HYDROFLUORIC ACID (HF) (or 20 ml of CoMat 01-132 HYDROFLUORIC ACID HF, 70 percent). Dilute to 1 l with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and mix well. Store in a plastic bottle.

       3. NOTE

          AR HF is an Analytical Reagent Trade hydrofluoric acid (48 to 51 percent).

          Optional synthetic standard solution (15 percent (that is, 150 ml/l) CoMat 01-327 NITRIC ACID), 0.5 percent (that is, 5 ml of CoMat 01-132 HYDROFLUORIC ACID HF/l = 7.3 ml AR/l) CoMat 01-357 HYDROFLUORIC ACID (HF) by volume.

          1. Continue as in Step (2).

       4. Ferrous sulfate solution (0.3N).

          1. Add 2600 ml (or 65 percent of the final volume) of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER to a 5 l Pyrex jar. With constant agitation, add very slowly 1000 ml (or 250 ml/l) of CoMat 01-320 SULFURIC ACID. Add 740 g (or 185 g/l) of CoMat 01-358 FERROUS SULFATE (FeSO4.7H2O), agitate to dissolve and cool in cold water. Filter the solution through CoMat 01-353 FILTER PAPER, using a Buchner funnel. Dilute with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER to 4 l.

          2. Standardization of the ferrous sulfate solution. Refer to Steps C.(1)(a) thru (g) for nitric acid content. Use a 2.0 ml specimen of primary standard nitric acid from Step B.(1)(a) in the place of the unknown process solution in Step C.(1)(c). Do again until 3 results are obtained.

             N = (NA x VA)/VF.

             where:

             N = Normality of ferrous sulfate.

             NA = Normality of acid.

             VA = Volume of acid.

             VF = Volume of ferrous sulfate - 0.2.

             Ferrous sulfate factor = N (ferrous sulfate) x 5.

          3. Do a check of the standardization and factor each week (or when needed if used less often) by treating primary standard acid and synthetic standards as unknowns and find nitric acid and hydrofluoric acid values along with production specimens.

       5. Sodium hydroxide (approximately 2N, 82.5 g/l).

          1. NOTE

             You can use a graduate or marked bottle because the solution is standardized against a primary standard.

             Dissolve 660 g of CoMat 01-314 SODIUM HYDROXIDE (NaOH), REAGENT GRADE (SOLID) in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 8 l.

          2. Standardize against primary standard nitric acid. (Refer to Step, Step 5.B.(2)). Use 30.0 ml portions of nitric acid solution and sufficient bromthymol blue indicator solution to produce a deep orange color.

          3. Calculations.

             Calculate individual normalities and average the individual results using the formula:

             N NaOH = (ml standard acid x N standard acid)/ml NaOH.

       6. Bromthymol blue indicator solution to use:

          1. Dissolve 0.10 g of CoMat 01-352 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED).

          2. Commerically prepared indicator is also available.

       7. 1000 ppM Titanium Atomic Absorption stock solution, Spex - (or equivalent).

    3. Procedure.

       1. Nitric acid content.

          1. Add 80 to 100 ml of CoMat 01-320 SULFURIC ACID to a 200 ml or 300 ml plastic beaker and a flat circular magnetic stirring bar if a magnetic stirrer is to be used.

          2. Place the beaker in an ice-cooled air-agitated water bath, or other applicable cooling medium. This may be placed on a magnetic stirrer.

          3. Pipette a 2.0 ml specimen of the solution with the NALGENE pipette and a rubber bulb or auto pipette. Slowly deliver the specimen below the surface of the CoMat 01-320 SULFURIC ACID. Be sure that the pipette tip stays below the surface of the sulfuric acid until the titration is completed.

             During the delivery of the specimen, when the magnetic stirrer is not used, stir the acid solution by the constant movement of the tip of the pipette along the sides of the beaker. Keep in contact with the bottom of the beaker.

             When the magnetic stirrer is used, keep a maximum agitation without splashing acid or exceeding spinner compliance speed. Movement of the pipette is not necessary.

          4. NOTE

             Temperature must not exceed 120 deg F (49 deg C) during titration. Standards and test specimens must be titrated in the same manner.

             Add ferrous sulfate solution (0.3N) in a fine stream to the mixture near the outer wall until the yellow color that first forms takes on a faint brown tinge. Keep a constant movement at all times in an applicable manner.

          5. Flush the pipette several times by sucking up the mixture to the marking with the rubber bulb. Permit it to drain back into the beaker.

          6. To complete titration, add the ferrous sulfate solution (0.3N) drop by drop; constantly stir until a yellow-brown color again appears (no more than two drops past the first appearance of color regardless of color intensity).

          7. Record the titer for nitric acid acidity.

       2. Ammonium bifluoride or Hydrofluoric acid content.

          1. NOTE

             For Solution Code 33, a 5.0 ml specimen may be used.

             Pipette a 10.0 ml specimen into a 400 ml plastic beaker. Add 175 to 200 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Stir well and add a magnetic bar and sufficient bromthymol blue indicator solution to produce a deep orange color.

          3. NOTE

             The indicator will not change to clear blue when selected solution has been in use. The yellow color will change to green and then gradually change to a solid opaque blue.

             Iron contamination will mask the end point, but the color may be seen at an angle through the edge of the solution. Stopping the agitation to permit the settling of brown precipitate after each sodium hydroxide addition also helps.

             Titrate with a 2N of sodium hydroxide solution with the use of strong agitation until traces of bluish color appears. Then slowly continue titration dropwise until the blue color continues at least one minute after the last drop has been added.

          4. Record the titer as total acidity.

       3. Titanium content in hydrofluoric-nitric acid process solutions: Wet chemical tests - Atomic absorption.

          1. Summary of method: Specimens are aliquoted from various tanks. The solution is aspirated into a nitrous oxide flame where the specimen is dissociated into atoms. Absorbance of the unknowns is compared to known standards. The concentration of titanium, in g/l, is then determined either instrumentally or manually.

          2. Standard preparation: Volumetrically pipette these various quantities of 1000 ug/ml titanium stock solution into a separate 100 ml volumetric flask and bring to volume with water and shake vigorously:

             For flask 1 the standard concentration of 0 ug/ml equivalent to 0.0 g/l for each ml of 1000 ug/ml Ti stock solution is 0.0.

             For flask 2 the standard concentration of 20 ug/ml equivalent to 2.0 g/l for each ml of 1000 ug/ml Ti stock solution is 2.0.

             For flask 3 the standard concentration of 50 ug/ml equivalent to 5.0 g/l for each ml of 1000 ug/ml Ti stock solution is 5.0.

             For flask 4 the standard concentration of 100 ug/ml equivalent to 10.0 g/l for each ml of 1000 ug/ml Ti stock solution is 10.0.

             For flask 5 the standard concentration of 125 ug/ml equivalent to 12.5 g/l for each ml of 1000 ug/ml Ti stock solution is 12.5.

             For flask 6 the standard concentration of 150 ug/ml equivalent to 15.0 g/l for each ml of 1000 ug/ml Ti stock solution is 15.0.

             For flask 7 the standard concentration of 200 ug/ml equivalent to 20.0 g/l for each ml of 1000 ug/ml Ti stock solution is 20.0.

          3. Specimen preparation: Volumetrically pipette 10 ml of specimen into a 1000 ml volumetric flask. Fill to volume with water and shake vigorously. Alternatively, pipette 1 ml of specimen with an Eppendorf pipette into a 100 ml volumetric flask and shake.

          4. NOTE

             Instrument is calibrated to read the final answer in g/l only for 10 to 1000 (or 1 to 100) dilution. If a different solution is used, do the alternate step that follows.

             Determination of titanium content: Set the instrument parameters as follows and make adjustments as necessary to maximize absorbance:

             Wavelength: 365.3 nm.

             Alternate wavelength: 320.0 nm.

             Slit opening: 0.2 nm.

             Operational mode: Abs AA-BG.

             Flame gases: Nitrous oxide and acetylene.

             Burner head: Nitrous oxide.

             Burner orientation: Normal.

             With the absorbance maximized, aspirate the 15.0 g/l standard.

             Switch operational mode (signal) to CONC (concentration).

             Enter 15.0 on the keyboard - (display reads 15.0, keyboard light on). Press key S1 once - (display reads 15.0, S1 light on). If so equipped, magnetic cards can be used to complete this step.

             Press key S1 once.

             Aspirate the standards and record the concentration in grams/liter (g/l).

             Aspirate the diluted test specimen from step (c) and record Ti concentration in g/l.

             Alternate step: Aspirate standards and specimens and record the readings. Maintain operational mode (signal) on ABS (absorbance). Absorbance reading must not exceed 0.466 units.

             Plot the standards curve on rectangular coordinates (concentration versus absorbance) or calculate a least square curve. This curve must be treated as linear only within the range established by the standards.

    4. NOTE

       All calculations corrected to equivalents of 10 ml specimen and 1.0N sodium hydroxide (10 Meq).

       Meq is the abbreviation for Molar Equivalent.

       To determine acid factors, refer to the NOTE in Test Method P-1, Step D. Refer to Step.

       Calculations.

       1. Nitric acid.

          Volume percent HNO3 = (Meq nitric acid/10ml) x (0.634)*.

          * The factor will vary with the type and quality of nitric acid.

          where:

          Meq HNO3/10ml = (Titer FeSO4 - 0.2) x (FeSO4).

       2. Ammonium bifluoride.

          Ammonium bifluoride oz/gal =.

          (Meq Total Acid/10ml)x(0.76 oz)/gal Meq.

       3. Hydrofluoric acid (70 percent).

          For 5 ml specimen,

          Vol percent HF acid =((Meq Total Acid - Meq HNO3)/10ml) x (0.49).

          For 10 ml specimen,

          Vol percent HF =.

          ((Meq Total Acid - Meq HNO3)/10ml) x (0.24).

          where:

          Meq Total Acid/10 ml = NaOH titer x N NaOH.

       4. Titanium.

          1. Refer to Fig Figure.

25. SUBTASK 70-11-47-180-024 Test Method P-36, Alkali Smut Removal Solution (Solution Code 47)

    1. Solutions.

       1. Silver nitrate (0.25M).

          1. Weigh 42.47 g of CoMat 01-360 SILVER NITRATE (AgNO3) dried at 205 to 215 deg F (96 to 102 deg C) for 1 to 2 hours, into a 1 l volumetric flask, dissolve in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and make up to volume. Store in an amber or dark glass container.

          2. Standardize - silver nitrate solutions, refer to Step, Step 5.B.(5).

       2. Sulfuric acid (0.5N).

          1. Add 14 ml of CoMat 01-320 SULFURIC ACID to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool and dilute to 1 l in a volumeter flask with water.

          2. Standardize, refer to Step, Step 5.B.(2).

       3. Gum arabic solution (10 percent).

          1. Dissolve 50 g of CoMat 01-354 GUM ARABIC in 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       4. Methyl red indicator solution.

          1. Dissolve 5.0 g of CoMat 01-064 INDICATOR (acid type formula C15H15N3O2 Formula weight 269.3) in 500 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED).

       5. Phenolphthalein indicator solution.

          1. Dissolve 1.0 g of CoMat 01-011 INDICATOR in 1 l of CoMat 01-239 ETHYL-ALCOHOL (DENATURED).

       6. Mixed indicator solution.

          1. Mix three parts phenolphthalein indicator solution and one part methyl red indicator solution.

    2. Procedure.

       1. Sodium cyanide (free).

          1. Pipette a 5 ml sample of solution into a 250 ml flask.

          2. Add 10 ml of gum arabic solution (10 percent) and 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          3. Titrate slowly with silver nitrate (0.25M) to a slight permanent turbidity.

       2. Activator.

          1. To the specimen from Step B.(1)(c), add 10 ml of silver nitrate solution (0.25M).

          2. NOTE

             Mixed indicator solution is necessary for a solution which has been in use and gives an advance warning to the final endpoint.

             Add 2 ml of methyl red indicator solution or 3 to 5 ml of mixed indicator solution.

          3. Titrate with a 0.5N sulfuric acid solution until the color changes from pink to cloudy white. Add 2 to 3 ml of methyl red indicator solution and titrate dropwise until the solution changes to faint pink.

          4. Record the titer.

          5. Make the solution basic after analysis with a few milliliters of strong caustic solution.

    3. Calculations.

       In these calculations NaCN means sodium cyanide and AgNO3 means silver nitrate.

       1. Sodium cyanide.

          1. Oz/gal NaOH = (ml AgNO3)(Molarity AgNO3)(2.62).

       2. Activator.

          1. For CoMat 01-143 ALKALI SMUT REMOVAL COMPOUND:

             Oz/gal activator = (ml H2SO4)(Normality H2SO4)(1.66).

26. SUBTASK 70-11-47-180-025 Test Method P-55, Caustic Soda or Potassium Permanganate

    1. Solutions.

       1. Sulfuric acid (1.0N).

          1. Add 28.0 ml of CoMat 01-320 SULFURIC ACID to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, cool and dilute to 1000 ml.

          2. Standardize - acid solutions, refer to Step, Step 5.B.(2).

       2. Sulfuric acid (1-1).

          1. Add slowly 400 ml of CoMat 01-320 SULFURIC ACID to 400 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER with constant agitation.

       3. Potassium iodide solution (10 percent).

          1. Dissolve 100 g of CoMat 01-308 POTASSIUM IODIDE (KI) in 1 l of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and add 1.0 g of CoMat 01-322 POTASSIUM HYDROXIDE. Store in a dark container.

       4. Starch solution.

          1. Purchase ready to use, or make a paste of 1.0 g of CoMat 01-385 STARCH with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 150 ml of hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and boil for 2 to 3 minutes. Store in a dark container.

       5. Sodium thiosulfate (0.1N).

          1. Dissolve 25.0 g of CoMat 01-383 SODIUM THIOSULFATE in 1 l of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Add 0.1 g of CoMat 01-382 SODIUM CARBONATE for each liter of solution and let it stand for one week.

          2. Standardize - sodium thiosulfate, refer to Step, Step 5.B.(4).

    2. Procedure.

       1. Alkalinity.

          1. Heat a sample solution slowly to 140 to 160 deg F (60 to 71 deg C); stir to mix.

          2. Add 5 ml of CoMat 01-381 METHYL ALCOHOL or 30 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED) to a 400 ml beaker. Pipette a 5 ml sample of the solution into the beaker and agitate until completely brown.

          3. NOTE

             Use CoMat 02-206 INDICATOR PAPER or CoMat 02-207 INDICATOR PAPER for pH determination.

             Add 75 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and one half a 3.85 cm ashless CoMat 02-208 FILTER PAPER TABLETS-ASHLESS or CoMat 02-189 COMPRESSED PAPER; then filter through a folded CoMat 02-205 FILTER PAPER into a 800 ml beaker. Wash well with hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER until the pH of the filtrate, on discharge from the funnel, is below pH 8.

          4. Add 2 to 3 drops of phenolphthalein solution to the filtrate (Refer to Step Step 5.A.(11) and titrate quickly to the colorless end point with a 1.0N sulfuric acid solution.

          5. Record the titer.

       2. Potassium permanganate.

          1. Heat a sample solution slowly to 140 to 160 deg F (60 to 71 deg C), stir to mix.

          2. Pipette a 25 ml sample into a 250 ml volumetric flask and dilute to the mark with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          3. Pipette a 10 ml aliquot specimen and transfer to a 250 ml beaker. Add 50 to 60 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          4. Add 10 ml of the 1-1 sulfuric acid solution and 25 ml of potassium iodide solution (10 percent).

          5. Titrate with 0.1N sodium thiosulfate to a light yellow color. Add 1 to 3 ml of starch solution and continue titration to the disappearance of the dark blue color.

          6. Record the titer.

    3. Sodium hydroxide and sodium carbonate.

       1. Procedure A.

          1. Continue as in Step B.(1), except cool to 35 to 45 deg F (2 to 7 deg C) after filtering in Step B.(1)(c).

          2. Record the titer as A.

          3. Add 2 to 3 drops of Methyl Orange indicator solution and continue to titrate to a faint pink end point (Refer to Step Step 5.A.(7)).

          4. Record the titer as B.

       2. Procedure B (Alternate).

          1. Pipette a 5 ml specimen into a 250 ml beaker.

          2. Add 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          3. Titrate quickly with a 1.0N sulfuric acid solution to a pH of 7.0 with a pH meter and automatic agitator.

          4. Record the titer as A.

          5. Continue to titrate to a pH of 3.5.

          6. Record the titer as B.

    4. Calculations.

       1. Alkalinity.

          Oz/gal sodium hydroxide = ml sulfuric acid x N sulfuric acid x 1.07.

       2. Potassium permanganate.

          Oz/gal KMn04 = ml Na2S2O3 x N Na2S2O3 x 4.2.

          where KMnO4 means potassium permanganate and Na2S2O3 means sodium thiosulfate.

       3. Sodium hydroxide and sodium carbonate.

          Oz/gal sodium hydroxide = (A-B) x N sulfuric acid x 1.08.

          Oz/gal sodium carbonate = 2B x N sulfuric acid x 1.43.

27. SUBTASK 70-11-47-180-026 Test Method P-59, Descaling Salt Bath

    1. Apparatus.

       Iron mortar and pestle.

       Crucible or other container of nickel or nickel alloy.

    2. Solutions.

       1. Hydrochloric acid (0.5N).

          1. Add 43 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool and dilute to 1 l with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER .

          2. Standardize - acid solutions, refer to Step Step 5.B.(2).

       2. Barium chloride (10 percent).

          1. Dissolve 1.0 g of CoMat 01-394 BARIUM CHLORIDE (BaCl2) in 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       3. Phenolphthalein indicator solution.

          1. Dissolve 1.0 g of CoMat 01-011 INDICATOR in 100 ml of CoMat 01-239 ETHYL-ALCOHOL (DENATURED).

    3. Procedure.

       1. Solution of sample.

          1. NOTE

             Salt is hydroscopic. Complete Steps (a) and (b) as quickly as possible.

             Break up the sample into large pieces with mortar and pestle.

          2. Weigh a 20 to 30 g sample into a tared 150 ml beaker.

          3. Dissolve with less than 400 ml of warm 120 to 130 deg F (49 to 54 deg C) CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER which has been previously boiled and cooled.

          4. Filter dissolved salts through folded CoMat 02-203 FILTER PAPER into a 1 l volumetric flask. Wash insoluble residue with warm CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Do this until the filtrate dropping from the funnel has a pH of 8 or less with CoMat 02-206 INDICATOR PAPER.

          5. Let the solution stand and cool for 16 to 24 hours.

          6. Filter again into another volumetric flask large enough to hold the solution and washings (1 l or 2 l). Wash again with cold (boiled and cooled) CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER until the filtrate is again below pH 8. Dilute to volume.

       2. Sodium hydroxide.

          1. Pipette a 25 ml sample from 1 l of clear solution, or a 50 ml sample from 2 l of clear solution, into a 250 ml beaker.

          2. Add 50 ml of boiled and cooled CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 20 ml of the barium chloride solution (10 percent). Stir and let it settle for 5 minutes.

          3. Add 5 to 10 drops of phenolphthalein indicator solution, with hydrochloric acid (0.5N) solution until a reddish-pink color disappears.

          4. Record the titer as A.

       3. Sodium carbonate.

          1. Pipette another sample as in Step (2)(a).

          2. Add 50 ml of boiled and cooled CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          3. Add 5 to 10 drops of phenolphthalein indicator solution, and titrate with hydrochloric acid (0.5N) solution until the reddish-pink color disappears.

          4. Record the titer as B.

    4. Calculations.

       In these calculations, HCl means hydrochloric acid, NaOH means sodium hydroxide, and Na2CO3 means sodium carbonate.

       1. Salt.

          1. Weight of salt x 0.025 = weight of salt in a 25.0 ml aliquoted sample.

          2. Weight of salt x 0.050 = weight of salt in a 50.0 ml aliquoted sample.

       2. Sodium hydroxide (NaOH).

          1. Titer A x Normality of HCl x 0.040 = g NaOH.

             Percent of NaOH = g NaOH x 100/weight salts (aliquot).

       3. Sodium carbonate.

          1. (Titer B - Titer A) x Normality of HCl x 2 x 0.053 = g Na2CO3.

             Percent of Na2CO3 = g Na2CO3 x 100/weight salts (aliquot).

             where HCl means hydrochloric acid and Na2CO34 means sodium carbonate.

28. SUBTASK 70-11-47-180-027 Test Method P-60, Hull Cell Testing

    1. NOTE

       Refer to the OPCI for supplier details.

       Apparatus.

       Hull cell, model WT, 267 ml capacity, thermostatically controlled.

       This can be obtained from:

       Supplier Code 02258 or Supplier Code 71361.

    2. Rectifier.

       Hull cell agitator - transverse - reciprocating motion.

       Panels of brass and steel.

       Anodes of cadmium and nickel.

       Stopwatch.

       Hull cell standard chart.

    3. Solutions.

       1. Additive stock solution.

          1. Add 334 ml of CoMat 01-349 CADMIUM PLATE BRIGHTENER to a 500 ml volumetric flask, add CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER to volume. Increment 1 ml = 1 quart for every 100 gal of solution being tested when used with a 267 ml Hull cell.

       2. Alkaline cleaner.

          1. CoMat 01-138 ALKALI CLEANER (HEAVYDUTY) or CoMat 01-139 ALKALI CLEANER (HEAVYDUTY) made to a concentration of 16 oz/gal.

    4. Procedure.

       1. Cadmium (for Brightener).

          1. Fill the Hull cell with the solution to be tested to the mark on the side of the cell.

          2. NOTE

             The make-up of a 1-1 hydrochloric acid solution is 1 volume of CoMat hydrochloric acid diluted with 1 volume of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

             After cleaning the cadmium anode in a 1-1 CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE, and rinsing, position the anode in the Hull cell.

          3. Keep the solution at room temperature.

          4. NOTE

             The make-up of a 1-1 hydrochloric acid solution is 1 volume of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE diluted with 1 volume of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

             Remove zinc from steel panels by putting them fully into a 1-1 hydrochloric acid solution and wiping the smut from the surface using a clean gauze cloth.

          5. Rinse in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and check for water breaks.

          6. Place the steel panel in the Hull cell.

          7. Position the agitator rod so it will pass by a full length of the cathode. The rod should be close to the face of the panel.

          8. Connect the leads from the rectifier to the panel and anode, positive to the cadmium anode, and the negative to the panel.

          9. Set the agitator to high speed.

          10. Turn on the power and run the test at 3 amps for 2 minutes.

          11. Remove the plated panel from the apparatus, then flush with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dry by dipping in CoMat 01-239 ETHYL-ALCOHOL (DENATURED) or CoMat 01-393 ACETONE and allow to stand until dry.

          12. Read the current density range from the furnished chart, refer to Fig Figure.

          13. To increase current density range, add 1 ml additive stock solution to cell, stir well. Refer to Step C.(1).

          14. Do the procedure again from Step (d) to (l) until you get the necessary brightness.

          15. Record the total addition of additive agent and ranges of current densities.

          16. Do not make more than 3 tests on one specimen of the solution to be tested.

       2. Nickel strike (Current Density).

          1. Fill the Hull Cell with solution to the correct level and keep at room temperature.

          2. Remove plastic film from the brass panel and put fully into 35 percent of hydrochloric acid solution for 5 to 10 seconds.

          3. Put fully in alkaline solution and anodically clean for 10 to 15 seconds. Remove and flush in hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Refer to Step C.(2) for the make-up of the alkaline cleaner solution.

          4. Place the panel in 35 percent hydrochloric acid solution and agitate for 5 to 10 seconds. Remove and flush in cold CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          5. Position the brass panel in the Hull Cell.

          6. Put the agitator rod into a position as to pass the full length of the cathode, running at low speed.

          7. Connect leads from the rectifier to the panel and anode, positive to the nickel anode and negative to the panel.

          8. Turn on the power and run the test at three amperes for five minutes.

          9. Remove the panel from the solution. Rinse in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, dip in CoMat 01-393 ACETONE, and allow to dry.

          10. NOTE

              To find the effectivness of CoMat 01-281 ACTIVATED CARBON or CoMat 01-282 ACTIVATED CARBON (GRANULAR) to be used in purification, 1 oz/gal of solution must be used and tested. Additional increments of activated carbon must be made until a panel is satisfactory to the requirements of Solution Code 30. You can use this finding to recommend the quantity of carbon to be used for purification of the production tank solution.

              Read the current density range from the furnished chart, refer to Figure, and record the results.

    5. Calculation for brightener.

       1. 1 qt/100 gallons = 1 ml of additive solution in 267 ml Hull Cell.

29. SUBTASK 70-11-47-180-028 Test Method P-66, Contractometer Determination of Nickel Plate Stress in Nickel Plate Solution (Solution Code 55)

    1. Apparatus.

       1. NOTE

          This contractometer is no longer manufactured; it is permitted to use this Witco product if you have one.

          Brenner-Senderoff Contractometer.

       2. NOTE

          This equipment (or use a unit with equivalent features and safeguards) is available from the sources that follow:

          Industrial Instruments, Inc.

          446 Winterhaven Drive,

          Newport News,

          VA 23606-2533 USA

          www.industrialinstruments.com

          Tel: +1-757-930-0856

          Fax: +1-757-930-3119

          Kameras Instruments

          10715 Clermont Avenue,

          PO Box 100

          Garrett Park, MD 20896 USA

          Tel: +1-301-946-3210

          Gearless Contractometer (refer to the manufacturer's instructions for its use).

       3. Additional helices for use with contractometer.

       4. Rectifier or other suitable DC current source with ammeter divisions of 0.1 ampere or smaller.

       5. Rack with nickel anodes for supporting contractometer. Refer to Figure.

       6. Bubble gage, which can be attached to the rack.

       7. Stopwatch, or other suitable timing device.

       8. Mandrel, 0.7495 to 0.7505in. (19.04 to 19.06 mm) outside diameter x 12in. (304.80 mm) long minimum.

       9. Ball micrometer.

       10. Rule, with suitable dimension units.

       11. Analytical balance.

    2. Measurement of helix. Refer to Fig Figure.

       1. Measure the outside diameter of the mandrel and record as (dm).

       2. Clamp one end of the helix onto the mandrel. Compress the turns gently so that they touch each other.

       3. Tighten the other clamp, of an equivalent width dimension as those to the fixture, to the end of the helix as positioned for measuring.

       4. Measure the distance between the clamps to the nearest 0.010in. (0.25 mm) and record as (L).

       5. Measure the pitch of the helix, the distance between windings, to the nearest 0.010in. (0.25 mm) and record as (P).

       6. Measure the outside diameter of the helix with a ball micrometer at five locations along the length. Take an average dimension and record as (dh).

       7. Loosen the clamp bolts and remove the helix from the mandrel.

       8. NOTE

          Optional - Measure thickness of the helix with a ball micrometer in five places and get an average.

          Calculate the thickness of the helix (t).

          t = (dh - dm)/2.

    3. Preparation of the helix.

       1. Degrease the helix. Refer to the SPM TASK 70-11-03-300-503.

       2. Clean anodically (reverse current) in Solution Code 39 for 10 to 30 seconds.

       3. Flush in running CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. If the helix shows visual water breaks when removed from the water, do the cycle again.

       4. Dry with reagent grade alcohol or CoMat 01-393 ACETONE.

    4. Determine of helix constant.

       1. Mount a prepared unplated helix onto the spindle of the instrument. The helix should be flush with the shoulder of the upper support mount A, refer to Figure, and even with the end of the lower support mount B.

       2. Install clamps over the helix at A and B and tighten to secure the helix to the mounts. Tighten screw S correctly for handling.

       3. Remove cover from the instrument dial; then use the bubble gage to level the instrument. The instrument can be set in an anode cage which has been leveled before. Refer to Fig Figure.

       4. Put the screw threaded end of the pulley arm into hole C, refer to Fig Figure. The pulley arm must be on the same plane as the dial face.

       5. Hang a looped thread over stud Q on sector and draw over the pulley.

       6. Accurately weigh a 1 oz weight to four decimal places (Record as wt).

       7. Attach the weight to the free end of the thread.

       8. Loosen set screw S and rotate the helix to bring stud Q into line with the pinion. Look at the alignment from the pinion gear to the sector gear (pinion gear centered on the sector gear).

       9. Slide the pulley on the bearing arm until the thread is perpendicular to the axial alignment of the contractometer gears (parallel to the pulley groove). Measure the distance between the arm and the center of the pulley in inches and record as (a).

       10. Check the helix for correct positioning, as in Step (1). Make sure that the helix in its fixed position has the same length as in the NO STRESS position and that the mechanism does not bind.

       11. If necessary, adjust the equipment; then tighten set screw S correctly.

       12. Lightly touch the dial face until you get a constant position of the dial pointer.

       13. Note this static position of the dial in degrees and record it as (W1).

       14. Remove the 1 oz weight, lightly touch the dial and record the new pointer position (W2). Calculate the deflection as (W).

           W = W1 - W2.

       15. Do the procedure again two more times. Calculate the average of the differences of the degrees deflection (W).

       16. Remove the pulley arm and thread and put the cover over the face of the dial.

       17. NOTE

           Constant determination must be done again after every 12 uses.

           Calculation of the constant of helix (K).

           K = (in x lb)/degree = ((wt) (a(in)) (0.002205 lb/gm))/W in deg.

           where.

           a = distance between the pulley and supporting arm (refer to Step D.(9)).

           wt = calibration weight (refer to Step D.(6)).

           W = degrees of deflection from calibration (refer to Step D.(15)).

    5. Calculation of plating current.

       AMPS = (45 (3.1416) (dh) (L))/144.

       where.

       45 = ASF (amperes/square foot).

       3.1416 = pi or the ratio of the circumference of a circle to its diameter.

       144 = Conversion factor (square inches/square foot).

       dh = outside diameter of helix (refer to Step B.(6)).

       L = height of helix (refer to Step B.(4)).

    6. Testing procedure.

       1. Helix preparation.

          1. Clean anodically in Solution Code 39 for 10 to 30 seconds at approximately 2 amp (30 to 40 ASF).

          2. Flush in running CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          3. NOTE

             A 20 to 30 percent hydrochloric acid solution has 20 to 30 volumes of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE hydrochloric acid for every 100 volumes of solution.

             Put fully into a 20 to 30 percent hydrochloric acid solution for 30 to 60 seconds.

          4. Flush in running CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Check for water breaks. Do Steps (a) thru (d) again until the helix shows no water breaks.

          5. Nickel strike in Solution Code 30 for 1 to 3 minutes at 4 to 6 amps.

          6. Flush in running cold CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and then in hot CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          7. Dry in an oven at 202 to 222 deg F (94 to 106 deg C), or dip in CoMat 01-031 ACETONE (CH3)2CO or CoMat 01-007 ETHYL ALCOHOL C2H5OH (DENATURED) and air dry.

          8. Weigh and record as (Bi).

          9. 

             CAUTION

             DO NOT DO STEPS (I) AND (J) IF THE HELIX USED HAS A PERMANENT TEFLON MASKING.

             Apply a mask or maskant to the helix with a thin even film of CoMat 02-021 MASKING WAX COMPOUND by putting fully into hot wax at approximately 200 °F (93 °C) until the helix is up to temperature, or mask the inside diameter of the helix with an even layer of CoMat 07-055 STOP-OFF LACQUER. Equivalent materials can be used. After application of wax, keep helix in constant rolling motion while cooling between absorbent towels to apply wax evenly over the inner surface.

          10. Let the helix cool and then remove all wax or lacquer from the outside diameter of the helix with a solvent that the wax or lacquer manufacturer specifies.

       2. Mounting and Cleaning Helix.

          1. NOTE

             Steel clamps must be lacquered or otherwise masked on the outside diameter surface. The lower clamp may be of plastic construction.

             Mount the helix on the spindle of the contractometer in a condition of NO STRESS and clamp in position. Pinion gear must be centered on the sector gear.

          2. 

             CAUTION

             DO NOT PERMIT ANY PART OF THE CONTRACTOMETER ABOVE THE UPPER CLAMP TO BECOME WET DURING THE STEPS THAT FOLLOW.

             

             CAUTION

             DO NOT PERMIT ANY SOLUTION TO ENTER THE ENCLOSED DIAL AREA OF THE APPARATUS.

             Clean anodically (reverse current) in Solution Code 39 for 10 to 30 seconds.

          3. Flush fully in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          4. NOTE

             A 20 to 70 percent hydrochloric acid solution has 20 to 30 volumes of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE for every 100 volumes of solution.

             Put fully into a 20 to 70 percent hydrochloric acid solution for 30 to 60 seconds.

          5. Flush fully in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Check for water breaks. Do Steps (b) to (e) again if necessary.

          6. Check the alignment of the pinion gear to the sector gear. Be sure that the assembled helix has free movement on the shaft of the apparatus.

       3. Plating procedure.

          1. If necessary, clean the anode cage. Follow the procedure given in Steps (2)(b) thru (2)(e).

          2. Use nonconductive supports to place arms of the fixture over the solution to be tested; then adjust the arms so that the solution will fully cover the helix. Mount the apparatus into the fixture that contains the nickel anodes. Refer to Figure. The solution must not be agitated too much. Let the helix and other components adjust to the solution temperature.

          3. Level the apparatus.

          4. Connect the positive lead to the nickel anodes and the negative lead to the steel clamp of the helix contractometer. Refer to Figure.

          5. Lightly touch the cover of the contractometer to get the initial position of the needle and record the readings for T = O,D = actual initial reading, at a density of 45 ASF.

          6. The test must be run at a serviceable current. The test time is 12 minutes at the current A, as calculated in Step E for the helix. When helix deflections show very high stress values, the test can be run for 20 minutes, or some other between time, but the minimum final calculated plate thickness must be 0.00037 in.

          7. Record the temperature of the solution, the elapsed total time of the test, the helix identification and the amperes used.

          8. Turn on the rectifier and increase current slowly to the predetermined amperage.

          9. NOTE

             Clockwise pointer movement indicates tensile values. Counterclockwise pointer movement indicates compressive values.

             Record the reading and find the deflection (D), each minute (T) for the duration of the test. Lightly touch the cover opposite the pointer before you obtain the readings.

          10. At the end of determination, disconnect the apparatus and remove from the plating solution. Flush in cold CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER; then flush in warm CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and blow dry.

          11. Loosen the clamps and remove the helix from the spindle.

          12. Remove masking from the inside diameter of the helix by degreasing or by the use of a suitable solvent. Air dry. Check for completeness of cleaning. Do Steps (j) and (l) again until clean.

          13. Place in desiccator. Weigh and record as (Bf).

          14. In preparation for next analysis, strip the nickel from the helix by putting fully in 1-1 nitric acid solution (that is, 1 volume of CoMat 01-327 NITRIC ACID mixed with 1 volume of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER) at 160 to 180 deg F (71 to 82 deg C). Flush fully. The chemically clean surface can now be processed through nickel strike as in Step F(1)(c) thru F(1)(g).

    7. .

       Stress calculation by formula.

       1. Calculate the deposit thickness (Dt) as follows:

          Deposit thickness (Dt) = (Bf-Bi)/(145.84) (3.1416) (dh) (L).

          where.

          (Bf-Bi) is in grams (refer to Steps F.(3)(m) and F.(1)(h)).

          145.84 is the conversion factor of density of nickel 8.9 g/cu cm to 145.84 g/cu in.

          3.1416 = pi or the ratio of the circumference of a circle to its diameter.

          dh = outside diameter (refer to Step B.(6)).

          L = length of plated area (refer to Step B.(4)).

       2. Calculate time (T) to two decimal places at which the plate was 0.0003in. thick.

          T/Total Test Time = 0.0003in./Deposit Thickness (Dt).

       3. Calculate (D) to the nearest tenth of a degree as follows and record.

          1. Interpolate T into the table of values recorded in time minus deflection records and record.

          2. Deflection (D) = interpolated value minus initial reading. Refer to Step F.(3)(e).

       4. Calculate stress (psi) and record.

          Stress (psi) = 2KD/tp (0.0003).

          where:

          t = thickness of helix (refer to Step B.(8)).

          p = pitch of helix (refer to Step B.(5)).

          D = calculate deflection for 0.0003in. (refer to Step G.(3)).

          K = helix constant (refer to Step D.(17)).

    8. Reference.

       1. H. Brenner and S. Senderoff, Procedure of American Electroplaters Society, 35-53 (1948).

30. SUBTASK 70-11-47-180-029 Test Method P-79, Acid Salt Solution

    1. Solutions.

       1. Sodium hydroxide (1.ON).

          1. Dissolve 40 g of CoMat 01-314 SODIUM HYDROXIDE (NaOH), REAGENT GRADE (SOLID) in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1 l with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Sodium hydroxide standardization, refer to Step Step 5.B.(1)(b).

    2. Procedure.

       1. Dry acid salt concentration.

          1. Pipette a 20 ml sample into a 250 ml flask.

          2. Add 75 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 8 to 12 drops of Bromcresol green indicator solution, refer to Step Step 5.A.(2).

          3. NOTE

             After continued use of a solution, the end point can be masked and the resultant end point would be considered a greenish blue.

             Titrate with sodium hydroxide solution (1.ON) to a permanent blue end point.

          4. Record titer.

    3. Calculations.

       1. Oz/gal dry acid salt = a x b x F.

          where.

          a = ml of sodium hydroxide solution.

          b = N of sodium hydroxide solution.

          F = factor as derived below.

    4. Derivation of factor.

       1. Weigh portion of salt that represents the highest concentration normally used.

          gm of salt (g) = 0.75 x concentration of salt desired.

       2. Dissolve in 75 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 100 ml.

       3. Pipette three 20.0 ml samples into 250 ml flasks. Titrate as given in Steps B.(1)(b) to B.(1)(d).

       4. Determine the average of the three values obtained.

          Factor = F = s/bc.

          where.

          s = concentration of acid salt.

          b = ml titer.

          c = normality of titrant.

31. SUBTASK 70-11-47-180-030 Test Method P-82, pH Determination

    1. Apparatus.

       pH meter.

    2. Solutions.

       1. Buffer solutions as necessary.

    3. Procedure.

       1. General instrument and installation instructions.

          1. Assemble to manufacturers instructions.

          2. Adjust and standardize to manufacturers instructions. Use correct buffer solutions.

       2. Solution examination.

          1. Transfer a sufficient volume and magnetic bar into a satisfactory sized beaker and set the stirrer to moderate agitation.

          2. Place the electrodes in a specimen container.

          3. Turn the meter to READ to pH position and read the indicated pH value.

          4. Record.

          5. Flush the electrodes and put fully in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER when not in use.

    4. Alternate procedure.

       1. Instrument and installation adjustment, assemble to manufacturers instructions.

          1. Wash the electrodes with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and wipe with absorbent tissue or fully flush it.

          2. Set temperature compensator to room temperature.

          3. Balance meter with necessary balancing controls.

          4. Put the electrodes fully in a beaker or a satisfactory vessel that contains the buffer solution so that the tips of the electrodes are at least 0,250in. (6.35 mm) below the surface.

          5. Turn the meter controls to READ or the correct pH position and adjust the calibration knob until the pH meter indicates the same reading as the buffer used.

          6. Turn the meter controls to NEUTRAL or REFERENCE position and note the meter needle position for reference point.

          7. Remove the electrodes from the buffer solution, flush with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, wipe with paper tissue or fully flush.

       2. Solution examination.

          1. Place the electrodes in a sample container.

          2. Make sure that the meter needle is still at REFERENCE point. If not adjust the meter again.

          3. Turn the meter control to READ or pH position and read the needle position.

          4. Record the pH.

          5. Flush the electrodes and put fully in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER when not in use.

    5. pH Adjustment:

       1. If the solution is too alkaline:

          1. Transfer 200 ml, or a known amount (the larger the specimen size, the better) of solution into a 600-800 ml beaker.

          2. Dilute the appropriate acid to be used as follows:

             Dilute 10 ml of acid to 200 ml in a volumetric flask.

          3. Adjust the pH with the appropriate acid, dropwise from a burette, to decrease the pH as desired.

          4. Record the volume of acid used.

       2. If the solution is too acidic:

          1. Dissolve 10.0000 + 2.0000 g of the appropriate base in 100 ml water. Dilute to volume in a 200 ml volumetric flask. If the base is in liquid form, dilute 10:200 as in Step E.(b).

          2. Transfer 200 ml or a known amount of the tank specimen into a 600-800 ml beaker.

          3. Adjust the pH with the appropriate base, dropwise from a burette, to increase the pH as desired.

          4. Record the volume of base used.

    6. Calculations.

       (1) Gallons of acid to add =.

       vol. of acid used (ml)x(ATC)x(.05)/vol. of tank specimen (ml).

       (2) Gallons of base to add =.

       vol. of base used (ml)x(ATC)x(.05)/vol. of tank specimen (ml).

       (3) Pounds base to add =.

       vol. of base used x(0.417)x(ATC)/vol. of tank specimen (ml).

       Where ATC = actual tank capacity in gallons.

32. SUBTASK 70-11-47-180-031 Test Method P-90, Inhibitor Replenishment for Solution Code 57

    1. Apparatus.

       1. Copper strips 3 x 0.5000 x 0.0625 to 0.3333in. (76,20 x 12,70 x 1,59 to 8,47 mm) thick cut from soft tempered, annealed, bus bars drawn from electrolytic copper ingots or bars conforming to American Society for Testing Material (ASTM) B5.

       2. Polishing material: CoMat 05-152 SILICON CARBIDE PAPER.

    2. Solutions.

       1. CoMat 01-096 ELECTROLYTIC STRIPPINGSOLUTION - control solution: To 300 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, add 100 ml of Solution A and 100 ml of Solution B. Dilute to 500 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       2. Light duty alkaline cleaner for copper or brass.

       3. Deoxidizing solution: 30 to 50 percent hydrochloric acid.

          1. Add 250 ml of concentrated CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 200 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Dilute to 500 ml with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       4. CoMat 01-278 NICKEL STRIP ADDITIVE. Pipette 25 ml of purchased additive to a 100 ml volumetric flask. Dilute to volume with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

    3. Procedure.

       1. Polish two copper strips with CoMat 05-152 SILICON CARBIDE PAPER.

       2. Dip the copper strips in alkaline cleaner. Remove and flush fully in warm CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       3. Dip the copper strips in acid solution. Remove and flush fully in cold CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       4. Pour 50 ml of room temperature CoMat 01-096 ELECTROLYTIC STRIPPINGSOLUTION into a 100 ml beaker and 50 ml of test solution into another 100 ml beaker.

       5. Put a copper strip fully into each of the two solution for 10 minutes.

       6. Remove and flush the copper strips in clean running CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and air dry.

       7. Compare the copper strips with regards to brown film.

       8. If film from test solution is lighter than film from control, deletion of CoMat 01-278 NICKEL STRIP ADDITIVE is indicated and the test should be continued as follows:

          1. Add 1.0 ml of CoMat 01-278 NICKEL STRIP ADDITIVE and do Steps (1) to (7) again.

          2. If brown film still does not match film from control do Step (a) again with further 1.0 ml additions of CoMat 01-278 NICKEL STRIP ADDITIVE until brown film matches that from control.

    4. Calculations.

       Fl oz/gal of additive to add = ml additive used x 2.6 x 0.25.

       ml/gal of additive to add = Fl oz/gal to add x 29.57.

33. SUBTASK 70-11-47-180-032 Test Method P-91, Analysis of Nickel Strip Solution

    1. Solutions.

       1. Hydrochloric acid (0.5N).

          1. Add 43.0 ml of CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE to 500 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1 l with CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Mix well.

          2. Standardize, refer to Step Step 5.B.(2).

       2. CoMat 01-355 INDICATOR. Purchase ready to use.

    2. Procedure.

       1. Filter at least 150 ml to remove sludge.

       2. Pipette 5 ml of filtrate into a 250 ml Erlenmeyer flask, add approximately 50 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 1 ml of CoMat 01-355 INDICATOR.

       3. Titrate with the 0.5N hydrochloric acid solution against a white background (0.5 tablet of CoMat 02-189 COMPRESSED PAPER) .

          1. A new solution will change from green to purple.

          2. Older solutions will turn brown-red.

       4. Record the titer.

    3. NOTE

       To increase the value of CoMat 01-096 ELECTROLYTIC STRIPPINGSOLUTION, add 2 parts of Solution B to 1 part Solution A.

       Calculations.

       Percent strip = HCl solution titer x N of HCl solution x 1.133.

34. SUBTASK 70-11-47-180-033 Test Method P-100, Chlorides and Boric Acid in Nickel Plate Solutions

    1. Apparatus.

       1. pH meter and/or Fischer Accumet 750 or Orion 901 Ionalyzer or equivalent.

       2. Magnetic bar and stirrer.

       3. Silver indicating electrode and Reference electrode - (Fischer Catalogue No.13-639-122 and 09-313-216 respectively).

          or.

          Silver sulfide ion-selective electrode and Double-junction reference electrode - (Orion Catalogue No.941600 and 900200 respectively. Fill inner and outer chambers with No.900002 solution).

    2. Solutions.

       1. Silver nitrate (0.1M).

          1. Dissolve 16.9890 g of CoMat 01-360 SILVER NITRATE (AgNO3), dried before for 1 to 2 hours at 205 to 215 deg F (96 to 102 deg C), in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and dilute to 1 l. Store in a dark bottle.

          2. Standardize, refer to Step Steps 5.B.(5).

       2. Silver nitrate (0.01M).

          1. Pipette a 10 ml specimen of the 0.1M silver nitrate solution and dilute to 100 ml in a volumetric flask. Store in a dark container.

       3. Potassium chromate (10 percent).

          1. Dissolve 10.0 g of CoMat 01-321 POTASSIUM CHROMATE (CHLORIDEFREE) in 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

       4. CoMat 01-310 INDICATOR.

          1. As purchased, ready to use, 0.04 percent, pH 5.2 to 6.8 adjusted to pH 6.0.

       5. Sodium hydroxide (0.1M).

          1. Dissolve 4.0 g of CoMat 01-314 SODIUM HYDROXIDE (NaOH), REAGENT GRADE (SOLID) in CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Cool and dilute to 1 l.

          2. Standardize, refer to Step Step 5.B.(1).

       6. Nitric acid (10 percent).

          1. To 50 to 60 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER, slowly and cautiously add 10 ml of CoMat 01-327 NITRIC ACID and dilute to 100 ml.

    3. Procedure.

       1. Chlorides (Nickel plating solution).

          1. Pipette 10 ml of plating solution into a 250 ml flask. Add 50 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 10 to 15 drops of the potassium chromate solution (10 percent).

          2. Titrate with the silver nitrate solution (0.1M) until the first permanent brownish tint appears.

          3. Record titer.

       2. Chloride (Alternate Procedure - Potentiometer).

          1. Pipette 10 ml of plating solution (20 ml of CoMat 03-108 SULFAMATE NICKEL PLATING SOLUTION) into a 250 ml beaker.

          2. Add 150 to 175 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER and 5 ml of the nitric acid solution (10 percent).

          3. Put Fishers or Orion electrodes fully in solution and set Ionalyzer to read millivolts. Wait for reading to stabilize.

          4. Titrate with the silver nitrate solution (0.1M) in increments of 0.5 ml.

          5. The end point is an increase in potential of approximately 60 mv.

          6. All an excess of 0.5 ml of the silver nitrate solution (0.01M) to be sure the endpoint has been reached.

          7. Record the titer as indicated in (2)(e).

       3. Chloride (Potentiometric procedure for CoMat 03-131 SULFAMATE NICKEL REPLENISHING SOLUTION) .

          1. Pipette a 50 ml specimen into a 250 ml beaker.

          2. Add 5 ml of nitric acid solution (10 percent).

          3. Put selected electrodes fully into the solution and wait for the reading to stabilize.

          4. Titrate with the silver nitrate solution (0.01M) in increments of 0.5 ml.

          5. The endpoint is given when the greatest increase in potential occurs after the addition of the initial 1 ml of the silver nitrate solution (0.01M).

          6. Add an excess of 1 ml (in 0.5 ml increments) of the silver nitrate solution (0.01M) to be sure that the endpoint has been reached.

          7. Record titer as indicated in (3)(e).

       4. Chloride (as hydrochloric acid) for Nickel strike solution (Solution Code 30).

          1. Pipette a 2 ml test specimen of the solution into a 250 ml flask and add 50 to 100 ml of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER.

          2. Neutralize the solution with sodium hydroxide solution (0.1M), refer to Step B(5), to a yellow end point, use methyl orange as an indicator, refer to Step Step 5.A.(7).

          3. Add 10 to 15 drops of the potassium chromate solution (10 percent), refer to Step B.(3), and titrate with silver (0.1M) until the first permanent brownish tint appears.

          4. Record titer.

       5. Boric acid.

          1. Pipette 5 ml of plating solution into a 150 ml beaker.

          2. Add CoMat 02-191 ALCOHOL to make a thick paste.

          3. Add 15 to 25 drops of CoMat 01-310 INDICATOR and 1 tablet of CoMat 02-189 COMPRESSED PAPER.

          4. Titrate with the sodium hydroxide solution (0.1M) until color changes from green to blue. Use necessary caution to be sure that all paste is off the sides of the beaker and enters into the reaction.

          5. Record titer.

    4. Calculations.

       In these calculations, AgNO3 means silver nitrate, HCl means hydrochloric acid, NaOH means sodium hydroxide, and Ni means Nickel.

       1. Chlorides.

          oz/gal chloride in nickel plate = titer x M AgNO3 x 0.473.

          CoMat 03-108 SULFAMATE NICKEL PLATING SOLUTION:

          oz/gal chloride in the plating solution = titer x M AgNO3 x 0.237.

          CoMat 03-131 SULFAMATE NICKEL REPLENISHING SOLUTION:

          oz/gal chloride in the replenishing solution = titer x M AgNO3 x 0.0946.

       2. CoMat 01-015 BORIC ACID H3BO3.

          oz/gal CoMat 01-015 BORIC ACID H3BO3 boric acid = titer x M NaOH solution x 1.652.

       3. CoMat 01-363 HYDROCHLORIC ACID (HCl),REAGENT GRADE.

          ml/gal HCl =.

          ((titer x M AgNO3 x 2.37) - (oz/gal Ni x 1.21)) x 66 ml/oz.

35. SUBTASK 70-11-47-180-034 Replenishing of Plating Solutions

    1. After a solution has been analyzed and concentration of elements known, it is then an easy step to replenish the solution to the necessary operating limits.

    2. In all calculations to get the necessary addition subtract the quantity present from the quantity necessary.

    3. Tank capacities are given in gallons unless differently specified.

    4. Use the formulae that follow as aids to calculate necessary quantities necessary to replenish, or keep, solutions within specified operating limits.

       1. Acid solutions.

          1. Gallons of acid to be added =.

             percent by volume necessary x tank capacity/100

          2. Pounds of CoMat 01-414 AMMONIUM BIFLUORIDE to be added =.

             oz/gal ammonium bifluoride necessary x tank capacity/16

       2. Chromic acid solutions.

          1. Pounds of CoMat 01-023 CHROMIUM TRIOXIDE CrO3(CHROM.ACID) to be added =.

             oz/gal chromium trioxide necessary x tank capacity/16

       3. Chromium plating solution.

          1. Pounds of CoMat 01-023 CHROMIUM TRIOXIDE CrO3(CHROM.ACID) to be added =.

             oz/gal chromium trioxide necessary x tank capacity/16

          2. Milliliters of CoMat 01-043 SULFURIC ACID H2SO4 to be added =.

             oz/gal sulfuric acid necessary x tank capacity x 15

       4. Chromate conversion solution immersion.

          1. Pounds of CoMat 03-129 CHROMATE CONVERSION SALTS to be added =.

             oz/gal chromate conversion salt necessary x tank capacity/16

          2. Gallons of CoMat 01-099 HYDROCHLORIC ACID to be added =.

             fl oz of hydrochloric acid necessary x tank capacity/128

          3. To decrease pH = add CoMat 01-099 HYDROCHLORIC ACID hydrochloric acid by increments, after CoMat 01-099 HYDROCHLORIC ACID hydrochloric acid analysis.

          4. Pounds of CoMat 03-129 CHROMATE CONVERSION SALTS to be added =.

             oz/gal chromate conversion salt necessary x tank capacity/16

          5. Milliliters of CoMat 01-025 NITRIC ACID HNO3, TECHNICAL GRADE to be added = ml of CoMat 01-025 NITRIC ACID HNO3, TECHNICAL GRADE necessary x tank capacity.

       5. Cleaners or Caustic soda.

          1. Pounds of CoMat 01-300 ALKALI CLEANER (GENERAL PURPOSE), CoMat 01-339 ALKALI CLEANER (GENERAL PURPOSE) or CoMat 01-340 ALKALI CLEANER (GENERAL PURPOSE) to be added =.

             oz/gal alkali cleaner necessary x tank capacity/16

       6. Copper plate and strike solutions (cyanide).

          1. Pounds of CoMat 03-102 COPPER CYANIDE to be added =.

             oz/gal Cu metal necessary x tank capacity x 0.0875

          2. Pounds of CoMat 01-063 SODIUM CYANIDE NaCN to be added =.

             (oz/gal NaCN needed x tank capacity/16)+(lbs of CuCN to be added x 1.1)

          3. Pounds of CoMat 01-107 POTASSIUM CYANIDE KCN95% MIN to be added =.

             oz/gal KCN necessary x tank capacity + (lbs CuCN to be added x 1.6)/16

          4. Pounds of CoMat 01-063 SODIUM CYANIDE NaCN to be added.

             oz/gal sodium cyanide necessary x tank capacity/16

          5. Pounds of CoMat 01-107 POTASSIUM CYANIDE KCN95% MIN to be added =.

             oz/gal potassium cyanide necessary x tank capacity/16

          6. Pounds of CoMat 01-030 SODIUM CARBONATE Na2CO3 to be added =.

             oz/gal sodium carbonate necessary x tank capacity/16

          7. Pounds of CoMat 03-105 POTASSIUM CARBONATE to be added =.

             oz/gal potassium carbonate necessary x tank capacity/16

          8. Pounds of CoMat 01-022 SODIUM HYDROXIDE NaOH (SOLID) to be added =.

             oz/gal sodium hydroxide necessary x tank capacity/16

          9. Pounds of CoMat 01-129 POTASSIUM HYDROXIDE KOH KOH, or CoMat 01-130 POTASSIUM HYDROXIDE KOH, or CoMat 03-107 POTASSIUM HYDROXIDE KOH to be added =.

             oz/gal potassium hydroxide necessary x tank capacity/16

       7. Alkali smut removers.

          1. Pounds of CoMat 01-143 ALKALI SMUT REMOVAL COMPOUND to be added =.

             oz/gal activator necessary x tank capacity x 1.5/16

          2. Pounds of CoMat 01-063 SODIUM CYANIDE NaCN =.

             (oz/gal NaCN needed x tank capacity/16)-(lbs alkali smut remover added x 0.33)

          3. Pounds of CoMat 01-063 SODIUM CYANIDE NaCN to be added =.

             oz/gal NaCN (free) necessary x tank capacity/16

       8. Neutralizer (Caustic-cyanide).

          1. Pounds of CoMat 01-063 SODIUM CYANIDE NaCN to be added =.

             oz/gal sodium cyanide necessary x tank capacity/16

          2. Pounds of CoMat 01-022 SODIUM HYDROXIDE NaOH (SOLID) to be added =.

             oz/gal sodium hydroxide x tank capacity/16

          3. Pounds of CoMat 01-107 POTASSIUM CYANIDE KCN95% MIN to be added =.

             oz/gal potassium cyanide necessary x tank capacity/16

       9. Nickel strike solution.

          1. Pounds of CoMat 01-077 NICKEL CHLORIDE NiCl2+6H2O to be added = oz/gal nickel metal necessary x tank capacity x 0.25.

          2. Milliliters of CoMat 01-099 HYDROCHLORIC ACID to be added =.

             ml of hydrochloric acid/gal x tank capacity

          3. Gallons of CoMat 01-099 HYDROCHLORIC ACID to be added =.

             (ml of hydrochloric acid needed/gal) x tank capacity/3785

       10. Nickel strip solution.

           1. Pounds of CoMat 01-063 SODIUM CYANIDE NaCN to be added =.

              oz/gal sodium cyanide necessary x tank capacity/16

           2. Pounds of CoMat 01-178 NICKEL STRIP SALT, or CoMat 01-179 NICKEL STRIP SALT, or CoMat 01-180 NICKEL STRIP SALT, or CoMat 01-181 NICKEL STRIP SALT or CoMat 01-182 NICKEL STRIP SALT = 0.5 the quantity of CoMat 01-063 SODIUM CYANIDE NaCN.

       11. Nickel plate (sulfamate).

           1. Gallons of CoMat 03-131 SULFAMATE NICKEL REPLENISHING SOLUTION to be added =.

              oz/gal nickel metal necessary x tank capacity/20

           2. Pounds of CoMat 01-077 NICKEL CHLORIDE NiCl2+6H2O to be added = oz/gal chloride necessary x tank capacity x 0.21.

           3. Pounds of CoMat 01-015 BORIC ACID H3BO3 to be added =.

              oz/gal boric acid necessary x tank capacity/16

           4. To adjust the pH. Add CoMat 01-416 NICKEL CARBONATE, solution code 51, or CoMat 03-130 SULFAMIC ACID.

       12. Silver plate and strike solutions.

           1. Pounds of CoMat 01-415 SILVER CYANIDE to be added =.

              oz/gal silver metal necessary x tank capacity x 0.078

           2. Pounds of CoMat 01-107 POTASSIUM CYANIDE KCN95% MIN to be added =.

              (oz/gal KCN x tank capacity/16) + lbs AgCN to be added x 0.5

           3. Pounds of CoMat 01-129 POTASSIUM HYDROXIDE KOH (KOH), CoMat 01-130 POTASSIUM HYDROXIDE KOH or CoMat 03-107 POTASSIUM HYDROXIDE KOH to be added =.

              oz/gal potassium hydroxide necessary x tank capacity/16

           4. Pounds of CoMat 03-105 POTASSIUM CARBONATE to be added =.

              oz/gal potassium carbonate necessary x tank capacity/16

           5. Pounds of CoMat 03-103 POTASSIUM SILVER CYANIDE or CoMat 03-104 POTASSIUM SILVER CYANIDE to be added =.

              oz/gal silver metal necessary x tank capacity x 0.115

           6. Pounds of CoMat 01-107 POTASSIUM CYANIDE KCN95% MIN =.

              oz/gal potassium cyanide necessary x tank capacity/16

36. SUBTASK 70-11-47-180-035 Solution Index

    SOLN. CODE No.	NAME	PROPERTY OR CONSTITUENT	MINIMUM FREQUENCY	TEST METHOD
    1	Caustic- Potassium Permanganate Descaling Solution	Sodium Hydroxide Potassium Permanganate	Every 2 months Every 2 months	P-55
    2	Deleted
    3	Deleted
    4	Alkali Cleaner (General Purpose)	Total Alkalinity	Every 2 months	P-6
    27	Hydrochloric Acid Solution 30%	Hydrochloric Acid	Monthly	P-1
    28	Nitric Acid Solution 55%	Nitric Acid	Every 3 months	P-1
    29	Sulfuric Acid Solution 20%	Sulfuric Acid	Monthly	P-1
    30	Nickel Strike Solution	Nickel Metal Chloride Contaminants	Monthly Monthly Every 2 months	P-17 P-100 p-60
    31	Sulfuric Acid Solution 40%	Sulfuric Acid	Every 3 months	P-1
    32	Titanium Etching Solution	Nitric Acid Hydrofluoric Acid	Monthly Monthly	P-33 P-33
    33	Nitric- Hydrofluoric Acid Solution	Nitric Acid Hydrofluoric Acid	Every 2 weeks Every 2 weeks	P-33 P-33
    34	Sulfuric Acid Solution 10%	Sulfuric Acid	Monthly	P-1
    35	Sodium Hydroxide Solution 3%	Sodium Hydroxide	Every 3 months	P-6
    36	Hydrochloric Acid Solution 65%	Hydrochloric Acid	Every 3 months	P-1
    37	Sulfuric- Hydrofluoric Acid Solution 30%	Sulfuric Acid	Monthly	P-1
    38	Molten Salt Bath	Sodium Hydroxide Sodium Carbonate	Every 12 months Every 12 months	P-59
    39	Alkali Cleaner	Total Alkalinity	Every 3 months	P-6
    40	Chromium Plating Solution	Chromic Acid Sulfate	Every 2 weeks Every 2 weeks	P-22
    41	Chromium Strip Solution	Total Alkalinity	Monthly	P-6
    42	Chromium Plating solution	Chromic Acid Sulfate	Monthly Monthly	P-22 P-22
    43	Self-Regulating Chromium Plating Solution	Chromic Acid Sulfate	Every 2 weeks Every 2 weeks	P-22
    44	Nitric Acid Solution 20%	Nitric Acid	Every 2 weeks	P-1
    46	Acid Salt Solution	Dry Acid Salt	Every 6 months	P-79
    47	Alkali Cleaner Solution (Medium duty)	Total Alkalinity	Monthly	P-6
    48	Alkali Smut Remover Solution	Activator Free Sodium Cyanide	Monthly Monthly	P-36 P-36
    49	Alkali Cleaner Solution (Heavy duty)	Total Alkalinity	Every 2 months	P-6
    50	Descaling Solution	Hydrofluoric Acid Nitric Acid Titanium	Every 2 weeks Every 2 weeks Monthly	P-33 P-33 P-33
    51	Sodium Hydroxide Solution 11%	Total Alkalinity	Monthly	P-6
    52	Silver Strike Solution	Silver Metal Free Potassium Cyanide	Monthly Monthly	P-30 P-30
    53	Silver Plate Solution	Silver Metal Free Potassium Cyanide Potassium Carbonate Potassium Hydroxide	Every 2 months Every 2 months Every 2 months Every 2 months	P-14 P-14 P-14 P-14
    54	Nickel Strip Solution (Cyanide)	Free Sodium Cyanide	Every 2 weeks	P-18
    55	Soft Nickel Plating Solution (Sulfamate)	Nickel Metal Boric Acid Chloride pH Stress	Every 2 months Every 2 months Every 2 months Weekly Every 4 months	P-17 P-100 P-100 P-82 P-66
    56	Multiple Strip Solution (Cyanide)	Free Sodium Cyanide	Monthly	P-18
    57	Nickel Strip Solution (noncyanide)(For silver or copper alloy brazed parts)	Inhibitor Replenisher Nickel Strip Solution	Monthly Weekly	P-90 P-91
    58	Alkali Cleaner	Alkalinity	Monthly	**
    60	Nickel Strip Solution (Cyanide)	Free Sodium Cyanide	Every 2 weeks	P-18
    61	Nickel Strip Solution (Noncyanide)(For silver or copper alloy brazed parts)	Part II	As required	**
    62	Descaling Solution	Nitric Acid Addition Agent Titanium Metal	**	**
    63	Descaling Solution	Nitric Acid Addition Agent Titanium Metal	**	**
    64	Descaling Solution	Nitric Acid Addition Agent Titanium Metal	**	**
    65	Gold-Nickel Braze Strip Solution	Nitric Acid Part B	Monthly Monthly	** **
    66	Nickel Strike Solution	Nickel Metal Boric Acid Hydrochloric Acid pH	Every 2 months Every 2 months Every 2 months Weekly	P-17 Proc. A P-100 * P-82
    67	Stripping Solution	Solution A Compound B	Every 2 weeks Every 2 weeks	** **
    68	Nickel Strip Solution (Noncyanide) (For silver or copper brazed parts)	Solution A Compound B Regulator	As required As required As required	** ** **
    75	Alkali Cleaner (General purpose, low foam)	Total Alkalinity		**
    82	Hydrochloric Acid Solution 100%	Hydrochloric Acid	Weekly	P-1
    84	Copper Sulfate Strike Solution	Metallic Copper Free NaCN Rochelle Salt or Rocheltex Hydroxide Carbonate	Weekly Weekly Weekly Weekly Weekly	P-8 P-8 P-8 P-9 P-4
    85	Deleted
    86	Electroless Nickel Plating Solution	Nickel Metal pH	*** ***	** **
    87	Electroless Nickel Plating Solution	Nickel Metal pH Solution A Solution B	*** *** Every 2 weeks Every 2 weeks	**
    88	Chromic Acid Solution	Chromic Acid	Monthly	P-22
    89	High Speed Chromium Plating Solution	Chromic Acid Sulfate CoMat 03-338 HIGH SPEED CHROM. REPLENISHERSOL	Monthly Monthly Monthly	P-22 P-22 P-22
    136	Deleted
    137	Electrolytic Cleaner Solution (Without Phosphate and Cyanide)	Alkalinity	Monthly	**
    138	Chromium Plating Solution	Chromic Acid Sulfate	Monthly Monthly	P-22 P-22
    150	Hydrofluoric - Nitric Acid Solution	Hydrofluoric Acid Nitric Acid Titanium	Every 2 weeks Every 2 weeks Every 2 weeks	P-33 P-33 P-33
    151	Nitric - Hydrofluoric Acid Solution	Nitric Acid Hydrofluoric Acid	Every 2 weeks Every 2 weeks	P-33 P-33
    153	Deleted
    154	Electrolytic Cleaner Solution (Cyanide-Type Phosphate-Free)	Alkalinity	Monthly	**
    155	Electroless Nickel Plating Solution	Nickel Metal pH	*** ***	** **
    156	Alkali Smut Removal Solution	Alkaline Material Sodium Cyanide	Monthly Monthly	P-36 P-36
    170	Sulfuric Acid Solution - 30 percent	Sulfuric Acid	Three Months	P-1
    * TASK 70-33-27-330-501 SUBTASK 70-33-27-180-037 (Solution Code 66) ** Refer to Manufacturer's Instructions *** Before and during operation
    NOTE For a cross reference list of IAE solution code numbers to equivalent Party Company designations, see TASK 70-11-58-110-501, SUBTASK 70-11-58-110-501.

37. SUBTASK 70-11-47-180-036 Chromic Acid Solution Free Chromic Acid Titration (Test Method P-2)

    1. Apparatus

       1. pH meter.

    2. Solutions.

       1. Sodium hydroxide

          1. Dissolve 40.0 g of CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER. Dilute to 1000 ml with water.

          2. Let the solution become cool, then add sufficient CoMat 01-201 DISTILLED, DEIONIZED, DEMINERALIZED, OR REVERSE OSMOSIS (RO) WATER to increase the solution volume to 1000 ml.

          3. Standardize the solution. Refer to Sodium Hydroxide and Potassium Hydroxide Solutions in Step

    3. Procedure

       1. Free Chromic Acid (CrO3) and Total Hexavalent Chromium.

          1. Pipette 25.00 ml of anodizing solution into a 250 ml beaker and dilute to approximately 100 ml with water,

          2. With continuous stirring, titrate with NaOH (1.0N) to a pH of 3.2 on the pH meter, and record the burette reading as X. Continue to titrate the sample to a pH of 4.8, and record the burette reading as Y. Near each end point, add the NaOH solution cautiously, as small quantities of the NaOH solution will cause a large increase in pH.

    4. Calculations

       1. Oz/gal free chromic acid (CrO3) = X x (N of NaOH) x 0.53 where X = NaOH burette reading in ml at pH of 3.2, and N = normality of NaOH solution

       2. Oz/gal total hexavalent chromium = Y x (N of NaOH) x 0.53 where Y = NaOH burette reading in ml at pH of 4.8, and N = normality of NaOH solution

       3. Percent free chromic acid (CrO3) = X x (N of NaOH) x 0.4 where X = NaOH burette reading in ml at pH of 3.2, and N = normality of NaOH solution

       4. Percent total hexavalent chromium = Y x (N of NaOH) x 0.4 where Y = NaOH burette reading in ml at pH of 4.8, and N = normality of NaOH solution

Figure: Solution Index Fig 70-11-47-990-001

Solution Index Fig 70-11-47-990-001



Figure: Hull cell standard chart

Hull cell standard chart



Figure: Measure the helix

Measure the helix



Figure: Contractometer calibration

Contractometer calibration



Figure: Contractometer equipment

Contractometer equipment



Figure: Titanium calculations

Titanium calculations