CHELATING RESIN AMBERLITE XAD-16-1,5-DIPHENYL CARBAZIDE FOR PRECONCENTRATION AND SELECTIVE ANALYSIS OF CHROMIUM(VI)

Meyliana Wulandari*, M. Bachri Amran**

*Chemistry Study Program, Institut Teknologi Bandung **Analytical Chemistry Research Division, Institut Teknologi Bandung Jl. Ganesha No.10 Bandung, West Java, Indonesia 40132 OBJECTIVE
To develop and evaluate preconcentration and selective analysis method for Cr(VI) using chelating resin Amberlite XAD-16-1,5-Diphenylcarbazide with Flow Injection Analysis.

EXPERIMENTAL METHOD Synthesis of Azotized Amberlite XAD-16 PSDVB PSDVB-NO2 FT-IR PSDVB-NH2 Azotized PSDVB Evaluation : H2SO4 Concentration Contact Time Retention Capacity Eluen Concentration FIAAAS Azotized Amberlite XAD-16-DPC FT-IR

ABSTRACT Chromium (Cr) is widely used in various industries, such as for plating, tanning, paint and pigment production, and metallurgy which possibly contaminate the environment. Cr(III) compounds are one of the essential trace nutrients in human bodies, and play an important role in the metabolism of glucose and certain lipids, whereas Cr(VI) compounds are toxic and carcinogenic. The World Health Organization (WHO) regulated the permissible limit of 0.05 mg L-1 of Cr(VI) in wastewater. Consequently, the development of a sensitive and selective method of Cr(VI) is absolutely essential. The ion exchange resins have shown better metal ion retention, but with conventional resins the selectivity and preconcentration factors are relatively low. This problem can be overcome by covalently bonding of a suitable group to the supporting material. Amberlite XAD-16 functionalized with 1,5-Diphenyl carbazide chelating resin was synthesized, characterized and packed in minicolumn that was applied to preconcentration with flow injection analysis (FIA) and detected by Atomic Absorption Spectrometry. Preconcentration and selective analysis of Cr(VI) based on complex formation at H2SO4 0.05 M and eluted quantitatively with HNO3 5 M have been studied. In this research, the effect of H2SO4 concentration, contact time, retention capacity, eluent concentration were investigated. It was found that retention capacity is 2.24 mg Cr / g XAD and 24.71 g / g XAD for batch and dinamic method, respectively. The limit of detection obtained was 69 ppb and the precision was 3.68% at 95% confidence level. The FIA performance can be showed by enrichment factor, concentration efficiency, and consumptive index obtained was 2, 0.5 / minutes and 6.5 mL for 1 mL sample, respectively. Recovery percent of spike sample was ~100% at linear region of calibration curve between 100 900 ppb with a correlation coefficient was 0.985. The study of analytical and FIA performances showed that this method can be used to selective analysis of Cr(VI) on g / L level. 1. IR CHARACTERIZATION OF MODIFIED AMBERLITE XAD-16
mg / g

2. THE EFFECT OF H2SO4 CONCENTRATION

0,2100 0,25 0,2 0,15 0,1 0,05 0 0,2050 0,2000 0,1950 0,1900 0,1850 0,1800 0 0,02 0,04 0,06 0,08 0,1

3. CONTACT TIME

4. BATCH RETENTION CAPACITY

1,6 1,4 1,2 1 0,8 0,6 0,4 0,2 0 0 50 100 150 200 250 300 mg/g

Evaluation : Precision Limit of Detection Linierity % Recovery

FIA Performances Data Analysis

mg / g

0 10 20 30 40 50 60 70 80 90 100 110 120 Contact time (minutes)

Cr(VI) Concentration (ppm)

H2SO4 Concentration (M)

REFERENCE
Duran, C., Soylak, M., Bulut, V. N., Gundogdu, A., Tufekci, M., Elci, Latif., Senturk, H. B., (2007), Speciation of Cr(III) and Cr(VI) in Environmental Samples after Solid Phase Extraction on amberlite XAD-2000, Journal of the Chinese Chemical society, 54, 625634. Contact person : *liana_mey@yahoo.com ** bachriamran@yahoo.com

RESULT
The following results are taken from the selective analysis and preconcetration of Cr(VI) using chelating resin Amberlite XAD-16-1,5Diphenyl carbazide with Flow Injection Analysis and detected by Atomic Absorption Spevtrometry

6. THE EFFECT OF HNO3 CONCENTRATION

A.U

7. PRECISION
5,00 4,00 3,00 2,00 1,00 0,00 1 2 3 Repeatability 4 5 A.U 50 40 30 20 10 0 0

8. CALIBRATION CURVE

5. DINAMIC RETENTION CAPACITY

0,3 0,25 0,2 0,15 0,1 0,05 0 0 20 40 Time (second) 60 80 A.U Absorban

0,60 0,50 0,40 0,30 0,20 0,10 0,00 1 2 3 4 5

y = 0,047x - 0,705 R = 0,985 100 200 300 400 500 600 700 800 900 Cr(VI) Concentration (ppb)

HNO3 Concentration (M)

LOD = 69 ppb CONCLUSION

% Recovery ~100%

9. SAMPLE ANALYSIS AND RECOVERY %

Spike Measured 0,18 g/L Spike Calculated 0,18 g/L

Wastewater sample of PT. Pindad 85 ppb

The use of chelating resin Amberlite XAD 16-1,5 Diphenyl carbazide to preconcentration and selective analysis of Cr(VI) shows good results based on Analytical and Flow Injection Analysis performances.