Ammoni a Content, Ti trimetr ic

Test Method No.: 254800 (A13.0) Revision No.: 02

Principle of Test Measurement:

Determination of ammonia content (in percent) by means of an indirect titration with sulfuric acid.
The endpoint is detected visually or by using a pH-electrode.

Purpose and Application:

This test method is used to determine the ammonia content of a raw material.

Equipment:
The equipment listed in this section should be in proper working order, suitable for the analysis, and properly
documented as required by local operating procedures and/or regulations. The Raw Material or Product Data Sheet
should be reviewed to determine if specific test equipment is required to assay the sample material.

1. Automatic titrator (e.g. Metrohm Titrando 907) and pH-electrode (e.g. Schott N 61) or
appropriate burette for visual endpoint determination
2. 30ml volumetric pipette, Class A
3. Erlenmeyer Flask, 200 ml
4. Analytical Balance capable of weighing to a resolution of 0.0001g
5. Disposable syringe

Reagents and Solutions:

The materials listed in this section should be suitable for the analysis and properly documented as required by local
operating procedures and/or regulations. The Raw Material or Product Data Sheet should be reviewed to determine
if specific reagents or test solutions are required to assay the sample material.

1. 1.0N Sulfuric acid (e.g. VWR# BDH 7232-1) or an ampoule of 1.0N sulfuric acid (Titrisol,
Merck # 9981/0001) to be transferred to a 1 liter volumetric flask and diluted to the mark
with water.
2. 1.0N Sodium hydroxide (e.g. VWR# BDH 7222-1) or an ampoule of 1.0N sodium
hydroxide (Titrisol, Merck # 9956/001) to be transferred to a 1 liter volumetric flask and
diluted to the mark with water.
3. Mixed indicator No. 5 (e.g. Merck # 6130 or Merck Millipore# 1061300250)
4. Oxalic acid*2H2O (CAS No. 6153-56-6) for titer determination

Procedure:
The Raw Material or Product Data Sheet should be reviewed to determine if specific sample preparation is required
or if specific test parameters are stated.

1. Pipet exactly 30.0ml of 1.0N sulfuric acid into a 200 ml Erlenmeyer flask.
2. Approximately 2ml of the aqueous ammonia solution are added by using a disposable
syringe. In reweighing the syringe the sample amount (W, in g) is recorded to the
nearest 0.001g.
3. a) Manual Titration- A few drops of mixed indicator No. 5 are added and the solution is
titrated with 1.0N sodium hydroxide until the color changes from violet to green. Record
the amount of titrant consumed (V, in ml) to nearest of 0.01 ml.
Or
b) Automated Titration- Titrate with 1.0N sodium hydroxide until the equivalence point is
reached. An example for the instrument setting of the titrator is given in Appendix A

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 Ammoni a Content, Ti trimetr ic

Test Method No.: 254800 (A13.0) Revision No.: 02

Titer/Calibration/Standardization:

1. Titer determination for NaOH

Note: Check the titer of NaOH at least every second week.

a. Weigh approximately 400mg Oxalic acid*2H2O (W, in mg) to the nearest 0.1mg
into a 150mL beaker.
b. Add approximately 80mL of deionized water and dissolve completely. For manual
titration only, add a few drops of mixed indicator No. 5 to sample solution.
c. Titrate with 1.0N NaOH. Record the volume of titrant used (V, in ml) to the
nearest 0.01ml.
d. Calculate titer using equation 1.

W W
t (NaOH) =  (1)
1/2 * 126.07g/mol * 1.0mol/L * V 63,035 * V

W = sample weight in mg
V = consumption in ml
126.07 g/mol = molecular weight of oxalic acid*2H2O

2. Titer determination for H2SO4

Note: Check the titer of H2SO4 at least every second month.

a. Using a volumetric pipette, transfer 5.0ml of 1.0N H2SO4 into a beaker.

b. Add approximately 80ml deionized water. For manual titration only, add a few
drops of mixed indicator No. 5 to sample solution.
c. Titrate with 1.0N NaOH. Record the volume of titrant used (V, in ml) to the
nearest 0.01ml.
d. Calculate titer using equation 2.

V*t (NaOH)
t (H2SO4) = (2)
5

V = consumption in ml
5 = volume of 1.0N H2SO4 in ml

Evaluation/Calculations:
Any deviations from the procedure described in this document or in the associated Raw Material or Product Data
Sheet shall be reported together with the analytical result.

1. Calculate the amount of ammonia (%) in the sample using equation 3.

(30 * t(H2SO4) - V * t(NaOH)) * c * M * 100%

Ammonia (%) = (3)
W * 1000

Where;
30 = volume of sulfuric acid added (ml)

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 Ammoni a Content, Ti trimetr ic

Test Method No.: 254800 (A13.0) Revision No.: 02

V = volume of titrant consumed in the assay (ml)

c = concentration of the NaOH solution = 1.0 mol/L
M = molar mass of ammonia
W = sample weight (g)

Information in Raw Material or Product Data Sheet:

1. None

References:

1. Merck Standards, p.36

Comments:

1. Not Applicable

History/Changes:

1. Transferred to Harmonized format. (2014)

2. Correction of equation 1

Original Issue Date: 09.12.1974 Created by: Ms. Schaefer

Revision No / Issue Date: 02 / 11.08.2015 Revised by: Mathiesen/Huesgen

Appendix A

Example for the instrument setting of the titrator (Titrando 907, Metrohm):

1. Dynamic titration
2. Drift of measuring points: 50 mV/min
3. Frequency of measuring points: 4
4. Minimal increment: 10 µl
5. Potentiometric endpoint evaluation:
Endpoint criteria: 5

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