KBS021: Alpkem Recipes

Active

Replaces Alpkem Recipes

In use from 1988-01-01 to 2008-04-22

Abstract

Instructions for mixing and handling various Alpkem reagents.

Protocol

Follow all lab safety protocols when handling chemicals, including protective eye and skin wear and appropriate lab clothing.

Ammonium Reagents

Citrate Complexing Reagent (2L)

Sodium Citrate 63g

Sodium Hydroxide, Pellets 2 g

Nanopure Water

Brij 35 (30%) 20 ml

Partially fill a 2L volumetric flask with nanopure water. Add dry chemicals, stir until dissolved then bring to volume (2L) with nanopure water. Filter reagent. Store in refrigerator not longer than 6 weeks. To prepare working reagent add 5 ml Brij 35 / 1 Liter of solution. Prepare working reagent fresh daily.

Alkaline Phenol (.5 L)

Sodium Hydroxide (10N or 40% w/v) 40 ml

Liquid Phenol (88%) 47 ml

Nanopure Water

Partially fill a 500 ml volumetric flask with nanopure water. Place in ice bath and stir while slowly adding sodium hydroxide first, then liquid phenol. Dilute to volume (500 ml) with nanopure water and filter. Store refrigerated in light resistant container. This reagent should be made as needed and not stored more than 3 days.

NOTE: This reagent is hazardous waste! Any glassware, paper towels, gloves, filter paper, etc used/contaminated during this process must be treated or disposed of as hazardous waste.

Sodium Nitroferricyanide (1L)

Sodium Nitroferricyanide 0.5 g

Nanopure Water 1L

Partially fill a 1L volumetric flask with nanopure water. Carefully measure sodium nitroferricyanide and add to nanopure water. Bring to volume (1L) with nanopure water and filter. Store refrigerated in light resistant container not longer than 6 weeks.

NOTE: This reagent is hazardous waste! Any glassware, paper towels, gloves, filter paper, etc used/contaminated during this process must be treated or disposed of as hazardous waste.

Nitrate/Nitrite Reagents

Ammonium Chloride EDTA Buffer (4L)

Ammonium Chloride 340 g

EDTA 0.4 g

10N Sodium Hydroxide 20+ ml

Nanopure Water 4L

Brij 35 (30%) 8ml

Partially fill a 4L Erlenmeyer flask with nanopure water. Add ammonium chloride and EDTA and stir until dissolved. Adjust buffer solution using 10 N sodium hydroxide (start with 20 ml and add from there as needed) to pH 8.50. Dilute to volume (4 L) with nanopure water and filter. To prepare working reagent add 4 ml Brij 35 / 1 Liter of solution. Prepare working reagent fresh daily. Store refrigerated.

NOTE: Always keep some of the buffer available that does not have Brij 35 added to it. This is used when reactivating the cadmium reduction coil.

Color Reagent (1L)

Phosphoric Acid (85%) 100 ml

Sulfanilamide 40 g

N-1-Naphthylethylenediamine dihydrochloride 2g

Nanopure Water 1 L

Partially fill a 1.0 L volumetric flask with nanopure water. On stir plate, add phosphoric acid then dry chemicals. Stir until dry chemicals are dissolved. This can take several hours of stirring. Bring to volume with nanopure water and filter. Store refrigerated in light resistant container.

Cadmium Coil Reactivation Reagents

(see page 16 of The Flow Solution Nitrate/Nitrite Methodology)

Nanopure Water

0.5 N Hydrochloric Acid

2% Copper Sulfate

Ammonium Chloride EDTA Buffer (no Brij 35)

0.5 N Hydrochloric Acid (100 ml)

Hydrochloric Acid (37%) 4.9 ml

Nanopure Water

Partially fill a 100 ml volumetric flask with nanopure water. While stirring (and in the hood), slowly add the hydrochloric acid. Bring to volume with nanopure water.

2% Copper Sulfate

Copper Sulfate 20 g

Nanopure Water

Partially fill a 1.0L volumetric flask with nanopure water. Add copper sulfate and stir until dissolved. Bring to volume (1L) with nanopure water.

h3.Cartridge Cleaning Solutions

If there are problems with contamination in the cartridges the following solutions may be used to clean the interior and related tubing. It is not necessary to disconnect plumbing to do this.

Nitrate/Nitrite Cartridge

1N Sodium Hydroxide

1 N Hydrochloric Acid

Ammonium Cartridge

1N Sodium Hydroxide

1 N Hydrochloric Acid

1 N Sodium Hydroxide (1 L)

10 N Sodium Hydroxide 100 ml

Nanopure water

Partially fill a 1.0 L volumetric flask with nanopure water. While stirring (and in the hood), slowly add the sodium hydroxide. Bring to volume with nanopure water.

1 N Hydrochloric Acid (1 L)

Hydrochloric Acid (conc.) 82.5ml

Nanopure Water

Partially fill a 1.0 L volumetric flask with nanopure water. While stirring (and in the hood), slowly add the hydrochloric acid. Bring to volume with nanopure water.

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Amount of sodium citrate added to Citrate reagent changed

2% Copper Sulfate

Copper Sulfate 20 g

Nanopure Water

Partially fill a 1.0L volumetric flask with nanopure water. Add copper sulfate and stir until dissolved. Bring to volume (1L) with nanopure water.

h3.Cartridge Cleaning Solutions

If there are problems with contamination in the cartridges the following solutions may be used to clean the interior and related tubing. It is not necessary to disconnect plumbing t
o do this.

Nitrate/Nitrite Cartridge

1N Sodium Hydroxide

1 N Hydrochloric Acid

Ammonium Cartridge

1N Sodium Hydroxide

1 N Hydrochloric Acid

1 N Sodium Hydroxide (1 L)

10 N Sodium Hydroxide 100 ml

Nanopure water

Partially fill a 1.0 L volumetric flask with nanopure water. While stirring (and in the hood), slowly add the sodium hydroxide. Bring to volume with nanopure water.

1 N Hydrochloric Acid (1 L)

Hydrochloric Acid (conc.) 82.5ml

Nanopure Water

Partially fill a 1.0 L volumetric flask with nanopure water. While stirring (and in the hood), slowly add the hydrochloric acid. Bring to volume with nanopure water.

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