standard testing procedure Bronopol

Sorage Requirements:
Store protected from light and moisture.

Sampling:
Sample from each container / bag, if the consignment is of 03or less than three containers / bags. If the number of containers / bags is more than 03and are upto 100, sample at randomely using the formula root (n) +1 where n is the number of containers/bags in the consignment. For the consignment of more than 100 containers/bags, sample additional containers/bags for every 100 containers/bags and thereafter.Collect a minimum of 5g from each of the randomely selected containers/bagsinto indiviually no toxic, selfsealing transparent polyethylene bearing ‘Sample For Analysis’label kept in another transperent self sealing polythene bag.Afetr completion of sampling return rest sample on the same container. Collect control sample in Pet bottle/Glass bottle.

Quantity of Composite Sample:

10 g

Quantity of Control Samle:

2 X 10 g

Description: White or almost white crystals or crystalline powder.

Solubility: Soluble in water, ethanol (95 per cent), ethyl acetate. Slightly soluble in chloroform, acetone, ether and
Benzene.

Identification:
A. By IR: The infrared absorption spectrum of bronopol is concordant with the reference spectrum of bronopol RS.

B. By chemical: The resulting solution gives reaction A of bromides.

pH: 5.0 to 7.0

Related Substances: Determine by liquid chromatography
A) Any peaks corresponding to 2-methyl-2-nitropropane-1,3-diol and tris(hydroxymethyl) nitromethane: NMT
0.5% each.
B) The area of any other secondary peak is not more than the area of the principal peak in the chromatogram
obtained with reference solution(a).

Sulphated Ash: NMT 0.1 % w/w.

Water: NMT 0.5 per cent.

Assay: Between 99.0% to 101.0%w/w on the anhydrous basis.

Description: White or almost white crystals or crystalline powder.

Examine the individual samples by visually.

Reporting: Report as Complies/Does not comply.

Solubility:
Soluble in water : 1.0 g in 10 to 30 ml
Soluble in ethanol (95 %) : 1.0 g in 10 to 30 ml
Soluble in ethyl acetate : 1.0 g in 10 to 30 ml
Slightly soluble in chloroform : 0.1 g in 10 to 100 ml
Slightly soluble in acetone : 0.1 g in 10 to 100 ml
Slightly soluble in ether : 0.1 g in 10 to 100 ml
Slightly soluble in benzene : 0.1 g in 10 to 100 ml

Reporting: Report as Complies/Does not comply.

Identification:

A. Determine by infrared absorption spectrophotometry Compare the spectrum with that obtained with
Bronopol RS or with the reference spectrum of Bronopol.

Reporting: Report as Complies/Does not comply.

B. Dissolve 0.1g in 10 ml of water, add 10 ml of 7.5M sodium hydroxide and carefully with constant
Stirring and cooling, 0.5g of nickel-aluminum alloy. Allow the reaction to subside, filter and
Carefully neutralize with nitric acid. The resulting solution gives reaction A of bromides. The
Resulting solution gives reaction A of bromides.

Reporting: Report as Complies/Does not comply.

pH: 5.0 to 7.0, Determined on 1.0 per cent w/v solution.

Reporting: Report as value.

Related Substances: Determine by liquid chromatography

Test solution: Dissolve 0.2g of the substance under examination in 100 ml of mobile phase.

Reference solution (a): Dilute 5 ml of the test solution to 50 ml with the mobile phase. Further, dilute 1 ml of the solution to 100 ml with the mobile phase.

Reference solution (b): A solution containing 0.001 per cent w/v each of 2-methyl-2nitropropan -1, 3-diol and tris (hydroxymethyl) nitromethane in the mobile phase.
Reference solution (c): A solution containing 0.0002 per cent w/v each of 2-methyl -2-nitropropane -1, 3-diol, 2 –nitroethanol, sodium bromide and tris (hydroxymethyl)-nitromethane in the mobile phase.
Chromatographic system

– a stainless steel column 15cm x 4.6mm, packed with octadecylsilane bonded to porous silica (5µm),
– column temeperature.35°,
– mobile phase : a mixture of 189 volumes of water , 10 volumes of acetonitrile and 1 volumes of a 10 per cent v/v solution of orthophospheric acid, adjusting the pH to 3.0 using 2 M sodium hydroxide,
– flow rate.1ml per minute,
– Spectrophotometer set at 214nm.
– Injection volume. 20µl.
–
Inject reference solution (c) The test is not valid unless the resolution between the peaks corresponding to sodium bromide and tris (hydroxymethyl) nitromethane is at least 1.0 and the resolution between the peak corresponding to tris (hydroxymethyl) nitromethane and 2-nitroethanol is at least 1.5.

Inject the test solution; reference solution (a) and reference solution (b) Continue the chromatography for 3 times the retention time of the principal peak. In the chromatogram obtained with the test solution the area of any peaks corresponding to 2-methyl-2-nitropropane -1, 3-diol and tris (hydroxymethyl) nitromethane are not more than the area of the corresponding peaks in the chromatogram obtained with reference solution (b) (0.5 per cent each) and the area of any other secondary peak is not more than the area of the principal peak in the chromatogram obtained with reference solution (a).

Sulphated Ash:
Determined 1.0 gm sample in silica crucible ignite for 800ºC and cool add 1 ml of sulphuric acid or ignite & calculated ash.

Calculation:

% of Ash = Weight of residue x 100

Weight of sample

Reporting: Report in %.

Water: The water content is determined with suitable Karl Fischer apparatus.
Procedure: take about 30 to 40 ml of methanol in to titration vessel and neutralize the solvent with standard K.F. reagent, than accurately about 5.0 gm of sample and transfer in to titration vessel then titrate with K.F. reagent to end point.

Calculation:

% of water = V x F x 100

W x 1000

Where,
V=Volume of K.F. reagent consumed for titration.
F=Factor of K.F. reagent.
W=Weight of the sample taken.

Assay: In a flask fitted with a reflux condenser dissolve 0.4g in 15ml of water and add 15ml of 7.5M sodium hydroxide. Slowly, with caution, add 2 g of nickel-aluminum alloy through the reflux condenser, agitating the
flask whilst cooling under running water. Allow the mixture to stand for 10 minutes and boil for 1 hour. Cool
and filtrate under reduced pressure, washing the condenser, flask and residue with 150ml of water.
Combine the filtrate and washings, add 25ml of nitric acid and 40ml of 0.1M silver nitrate shake vigorously
and titrate with 0.1 M ammonium thiocyanate using ammonium Iron (III) sulphate solution as indicator .Carry out
a blank titration.

1 ml of 0.1 M silver nitrate is equivalent to 0.020g of C3H6BrNO4.

Calculation:

Titrate volume x Normality of 0.1M silver nitrate x 0.020 x 100 x 100

0.1x Spl. wt. x (100-LOD)

Reporting: Reporting as %.

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