Escolar Documentos
Profissional Documentos
Cultura Documentos
Experimental
All absorbance measurements were made using
Elico SL 177 scanning spectrophotometer with 1 cm
matched glass cells. All chemicals used were
analytical grade reagents. Oxygen-free water was
used for the preparation of solutions. This was
prepared according to ASTM specification by boiling
distilled water and then cooling it under nitrogen
atmosphere to keep it free of dissolved oxygen.
For the stock solution, 0.1017 g of hydrazinium
sulphate was dissolved in 250 mL of water to give a
stock solution equivalent to 100 mg/L of hydrazine.
Bromate- bromide mixture for bromine generation
was prepared by dissolving 0.05g of potassium
bromate and 0.5 g of potassium bromide and diluting
to 500 mL with water. To generate 28 ppm of
bromine stock solution, 20 mL of bromate-bromide
mixture was diluted to 100 mL. An aliquot of this
stock solution (50 mL) was transferred into a 100 mL
calibrated flask containing 40 ml of 4.25 M sulphuric
Spectrophotometric determination of
hydrazine using bromine and methyl red
Mary Georgea, K S, Nagaraja a,* & N Balasubramanianb
a
1622
NOTES
1623
50
1.5
10
100
10
100
a
Treated with HCHO solution before the addition of bromine
solution.
b
If it is in the form of NH3 (NH4OH) treat the sample with 1 mL
of 0.1 M H2SO4 before treating with bromine solution
c
Treated with 1 mL of 0.5% sulphamic acid before treating with
bromine solution.
d
Treated with 1 mL of 1000 ppm HCHO solution followed by 5
mL of 8 M sulphuric acid and 1 mL of 0.5% of sulphamic acid
and diluted to 25 mL prior to analysis. 10 mL of sample was
used for analysis.
1624
Sample
Added NH2NH2
(g)
Recovery of added
hydrazine (%)
Sample 1
2
2
2
99.0
100.0
100.5
Sample 2
2
2
2
Sample 3
2
2
2
2.98
4.96
2.95
4.95
2.99
5.00
2.97c(297) b
1.98
3.99
2.01
4.01
1.95
3.95
1.98c (198) b
1.98
3.97
2.05
4.05
1.96
3.95
2.00c (200) b
2.95
2.90
2.90
2.92c (292) b
1.95
1.93
2.00
1.96c (196) b
1.95
2.00
1.93
1.96c (196) b
100.5
100.0
100.0
99.5
100
99.5
Water samples were withdrawn at the entry point of the boiler on different days.
1 mL of the sample was diluted to 100 mL before analysis and one mL of the diluted sample was used for hydrazine determination.
c
Average of three determinations
b
References
1 Abbas Afkhami & Ali Reza Zarei, Talanta, 62 (2004) 559
2 Dadfarmia S & Dehghan K, Bull Korean Chem Soc, 25
(2004) 213
3 Ali A Ensafi & Naderi B, Microchem J, 56 (1997) 269
4 Ali A Ensafi & Rezaei B, Talanta, 47 (1998) 645
5 Ortega- Barrales P, Molina- Diaz A, Pascual- Reguera M I &
Capitn- Vallvey L F, Anal Chim Acta, 353 (1999) 115
6 Safavi A & Ensafi A A, Anal Chim Acta, 300 (1995) 307
7 Afkhami A & Afshar-E-Asl A, Anal Chim Acta, 419 (2000)
101.
8 Deepa B, Balasubramanian N & Nagaraja K S, Asian J
Chem, 17 (2005) 1140.
9 Skoog D A, West D M & Holler F J, Fundamentals of
Analytical Chemistry, 7thEdn, (Harcourt Asia Pvt. Ltd), 2001,
375.
10 Laitinen H A & Boyer K W, Anal Chem, 44 (1972) 920.