1

WP Maintenance

1.2 Chrome Solution Analysis Procedures

09/26/95
09/26/95

SERVICE LABORATORYWORK INSTRUCTIONS

B.F.
1
QLWI 4.10.53
B. FARKAS
DETERMINATION OF CHROMIC ACID

Purpose:

To describe the steps to be taken to determine the concentration of

chromic acid in chromium plating solutions.

Reagents: Distilled Water

Ammonium Bifluoride crystals
Concentrated Hydrochloric Acid
20% Potassium Iodide Solution-(200g/l + 1 g/l Potassium Hydroxide )
0.10 N Sodium Thiosulfate Standard Solution
Starch Indicator
Procedure:
1)

Pipette a 2 ml sample into a 100 ml volumetric flask, dilute to volume with

distilled water and mix.

2)

Pipette 10 ml of this dilution into a 250 ml Erlenmeyer flask.

3)

Dilute with distilled water to between 100 and 125 ml.

4)

Add one scoop of ammonium bifluoride crystals and 15 ml of concentrated

hydrochloric acid.

5)

Add 5 ml of 20% potassium iodide solution.

6)

Titrate with 0.10 N sodium thiosulfate standard solution to a straw colour,

add 5 ml of starch indicator and continue titration until the blue colour
disappears.

Calculation
Chromic Acid ( g/l ) = ( ml 0.10 N Sodium Thiosulfate titrated ) x 16.725

SERVICE LABORATORY
WORK INSTRUCTIONS
09/26/95
09/26/95

B.F.
QLWI 4.10.54

1 of 2
B. FARKAS

DETERMINATION OF TRIVALENT CHROMIUM

Purpose:

To describe the steps to be taken to determine the concentration of

trivalent chromium in chromium plating solutions.

Reagents: Distilled Water

Ammonium Bifluoride crystals
Concentrated Hydrochloric Acid
20% Potassium Iodide Solution- (200g/l + 1 g/l Potassium Hydroxide)
Sodium Peroxide
0.10 N Sodium Thiosulfate Standard Solution
Starch Indicator
Boiling Chips
Procedure:
1)

Pipette a 2 ml sample into a 100 ml volumetric flask, dilute to volume with

distilled water and mix.

2)

Pipette 10 ml of this dilution into a 250 ml Erlenmeyer flask.

3)

Dilute with distilled water to between 100 and 125 ml.

4)

Add about 1/2 gram of sodium peroxide and some boiling chips.

5)

Place on the hot plate and boil for between 20 and 30 minutes.

6)

Remove from hot plate and dilute to between 100 and 125 ml with distilled
water and allow to cool.

7)

Add one scoop of ammonium bifluoride crystals and 15 ml of concentrated

hydrochloric acid.

SERVICE LABORATORY
WORK INSTRUCTIONS
09/26/95
09/26/95

B.F.
QLWI 4.10.54

2 of 2
B. FARKAS

DETERMINATION OF TRIVALENT CHROMIUM

Procedure (continued):

8)

Add 5 ml of 20% potassium iodide solution.

9)

Titrate with 0.10 N sodium thiosulfate standard solution to a straw colour,

add 5 ml of starch indicator and continue titration until the blue colour
disappears.

Calculation:
To calculate trivalent chromium, the Determination of Chromic Acid work
instruction - QLWI 4.10.53 must have already been performed.
Trivalent Chromium (g/l) = ( titration for trivalent chromium - titration for chromic acid ) x 9.0

SERVICE LABORATORY
WORK INSTRUCTIONS
09/26/95
09/26/95

B.F.
QLWI 4.10.55

1
B. FARKAS

DETERMINATION OF SULFATE BY KOCOUR TEST

Purpose:

To describe the steps to be taken to determine the concentration of

sulfate in chromium plating solutions.

Reagents: Distilled Water

Kocour Solution A - 50% Hydrochloric Acid Solution - ( 500 ml/l )
Kocour Solution B - 20% Barium Chloride Solution - ( 200 g/l )
Procedure:
Note: CR-110 and CR-710 solutions need to be heated to operating temperature
prior to analysis.
1)

Filter sample through No. 1 filter paper, if necessary.

2)

Add 5 ml of kocour solution A to a centrifuge tube.

3)

Pipette 10 ml of sample into the centrifuge tube.

4)

Add 5 ml of kocour solution B to the centrifuge tube and stopper.

5)

Shake the tube for exactly one minute, then allow to stand for five minutes
in the centrifuge.

6)

Centrifuge the tube for 5 minutes at 1250 rpm 50.

7)

Remove the tube and tap the stem until the precipitate has a flat surface, read.

Calculations:
Sulfate ( g/l ) = ( Volume of precipitate ) x 1.5 (if Kocour tubes have no decimal, that is, the
major graduations are 1,2,3,4,5,6)Sulfate ( g/l ) = ( Volume of precipitate ) x 15 (if Kocour tubes
have a decimal, that is, the major graduations are 0.1,0.2,0.3,0.4,0.5,0.6)

SERVICE LABORATORY
WORK INSTRUCTIONS
10/05/95
10/05/95

B.F.
QLWI 4.10.59

1
B. FARKAS

METALLIC IMPURITIES BY ATOMIC ABSORPTION

Purpose:

To describe the steps to be taken to determine the concentration of

metallic impurities in chromium plating solutions.

Reagents: Distilled Water

Procedure:
1)

Pipette a 2 ml sample to a 100 ml volumetric flask. Dilute to the mark with

distilled water and mix.

2)

Pipette 5 ml of this dilution to a 100 ml volumetric flask. Dilute to the mark

with distilled water and mix. This represents a 1000X dilution.

3)

Obtain readings for required impurities using Atomic Absorption

Spectroscopy.

Calculation:
ppm reading from A.A. = g/l in Chromium plating solution