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Running Head: Nitrate and Phosphate in Soil Samples

The Determination of Nitrate and Phosphate in Aqueous Extract of Soil Samples by Ion Chromatography Emily J. Mellott
Department of Chemistry and Biochemistry, Messiah College, Grantham, USA *em1313@messiah.edu, Messiah College One College Avenue 5893, Mechanicsburg, PA 17055

Nitrate and Phosphate in Soil Samples

The Determination of Nitrate and Phosphate in Aqueous Extract of Soil Samples by Ion Chromatography
The nitrate and phosphate content of a regular soil sample and a compost soil sample were determined by analyzing the aqueous extract of the soil samples with ion chromatography. The nitrate content of the regular soil was found to be 0.1358 mg nitrate/g soil with a standard deviation of 0.02836 mg nitrate/g soil, and the nitrate content of the compost soil sample was found to be 0.4720 mg nitrate/g soil with a standard deviation of 0.01394 mg nitrate/g soil. The phosphate content of the regular soil was found to be 0.08227 mg phosphate/g soil with a standard deviation of 0.007725 mg phosphate/g soil , and the phosphate content of the compost soil sample was found to be 0.2533 mg phosphate/g soil with a standard deviation of 0.01163 mg phosphate/g soil. These results demonstrate that as far as can be determined from this method, the compost does serve to increase the available content of nitrate and phosphate in the soil.

Introduction: The chemicals in soil are essential for healthy plant growth. While different elements are required in greater or lesser quantities, a deficiency in one could harm the plants ability to grow. Nitrogen, phosphorous, and potassium are the elements required in the largest quantities by plants for healthy growth.1 This analysis takes into account nitrogen and phosphorous. These elements are available in different forms in the soil, but nitrogen is mainly taken up by plants in water and is in the forms of NO3- and NH4+, and phosphorous is mainly taken up by plants in water and is in the form PO43-, HPO42-, and H2PO4-. In this project, the analysis was performed with ion chromatography, and the anions of interest were NO3- and PO43- . Ion chromatography is widely used as a method for determining inorganic anions in environmental samples. One reason for this popularity is that ion chromatography can analyze multiple anions at once. In

Nitrate and Phosphate in Soil Samples addition, it was shown to give the same results as other wet chemistry methods in the determination of common anions.2 Fertilizers are commonly used to increase the amount of nutrients in the soil and thereby facilitate more plant growth. An alternative to fertilizer is compost. Composting reduces trash and enriches the soil.3 In this analysis, the content of nitrogen available as NO3- and the content of phosphorous available as PO43- in the aqueous extract of a sample of soil from a garden that had not received compost and a sample of soil that had been exposed to compost was assessed by ion chromatography. The goal was to discover whether the nitrogen and phosphorous available in these forms and determined by this method was greater in the compost sample than in the regular soil sample. Materials and Methods: Two soil samples were collected on the same day. One was taken from a garden that had never been exposed to compost. The other sample was taken from the same yard but near a compost bin. The samples were kept in plastic baggies for a time. Next, the soil samples were dried in an oven at approximately 100C for 2 hours. While the samples were drying, 4 standards of NO3- and PO43were prepared from a 100 ppm stock solution of the anions. The standard solutions had concentrations of 1, 4, 20, and 40 ppm. After drying, the soil was put through a 40 mesh sieve to remove small stones and large clumps of dirt. Next, four portions of approximately one gram each of the regular soil sample were precisely weighed and transferred into small beakers. Then, three portions of approximately one gram each of the compost sample were also weighed and transferred into small beakers. Fifty milliliters of doubly distilled water were added to each beaker. After that, all the beakers were

Nitrate and Phosphate in Soil Samples stirred with moderate heat for one hour. The samples cooled, and all the samples were gravity filtered into 100 mL volumetric flasks. The soil in the filter was rinsed with purified water three times. Finally, the volumetric flasks were diluted to the mark with doubly distilled water. One of the regular soil samples was spiked with 1 ppm of the anions. The filter paper allowed some particles through, so it was necessary to use a syringe filter to remove the extra particles. All the solutions were analyzed using ion chromatography. The instrument was a Dionex ICS-2100. Results and Discussion: The results from the ion chromatograph for individual samples are displayed in Table 1. The nitrate had a retention time of around 8.6 minutes, while the phosphate had a retention time of around 14.0 minutes. Peak areas were measured and related to concentrations. Figure 1 shows a sample chromatograph for the regular soil. The concentrations of the unknowns were calculated from the calibration curves of the four standards shown for nitrate in Figure 2 and phosphate in Figure 3. The average content of nitrate in the regular soil was 0.1358 mg nitrate/g soil, and the average content of nitrate in the compost soil was 0.4720 mg nitrate/g soil. The average phosphate content of the regular soil was 0.08227 mg phosphate/g soil, and the average phosphate content of the compost soil was 0.2533 mg phosphate/g soil. The standard deviations and 95 % confidence interval for these values are listed in Table 2. The nitrate and phosphate content of the compost soil was greater than the content in the regular soil. It was found that the amounts of nitrate and phosphate in the regular sample were significantly different at the 95 % confidence level to the amounts of nitrate and phosphate in the compost sample. A blank was analyzed, and the chromatograph showed a large drift, but no obvious peaks were observed at any point on the graph. The spiked sample of

Nitrate and Phosphate in Soil Samples regular soil gave a 135.6 % recovery for nitrate and an 87.74% recovery for phosphate. The nitrate peak on that particular chromatograph was not resolved from another peak of a contaminant. Therefore, the area calculated from the nitrate peak may have been greater than it actually was leading to a greater percent recovery. The lower percent recovery for phosphate indicates that there was something in the method that decreased the amount of phosphate in the spike. Further replicates would need to be done to establish a good percent recovery for this method. In conclusion, this analysis demonstrated that the nitrate and phosphate content of soil that can be extracted with water was greater in a sample that was exposed to compost than a regular soil sample. Future projects might include using a different extraction method to get out all available nitrate and phosphate or letting the samples stir for a longer period of time. In addition, the potassium content of the soil samples could be determined using another method.

Acknowledgements: I thank the Department of Chemistry and Biochemistry at Messiah College for their support in this work. Specifically, I thank Dr. Schaeffer for his advice and assistance in this project.

References: (1) Schmidt, J. Healthy Soils, Healthy Foods. Food & Nutrition, March/April 2013, pp. 12-13. (2) Jackson, P.E. Ion Chromatography in Environmental Analysis. In Encyclopedia of Analytical Chemistry; Meyers, R. A., Ed.; Wiley: Chichester, 2000; p 27792801.

Nitrate and Phosphate in Soil Samples (3) He, Z.; Yang, X.; Kahn, B. A.; Stofella, P. J.; Calvert, D. V. Plant Nutrition Benefits of Phosphorous, Potassium, Calcium, Magnesium, and Micronutrients from Compost Utilization. In Compost Utilization in Horticultural Cropping Systems; Stofella, P.J.; Kahn, B.A., Eds; CRC Press LLC: Boca Raton, 2001; Ch. 15, pp. 307-317.

Nitrate and Phosphate in Soil Samples Table 1. Data from Ion Chromatograph for Nitrate and Phosphate from Regular and Compost Samples. *indicates spiked sample.

1 Regular 2 Regular 3 Regular 4 Regular* 1 Compost 2 Compost 3 Compost

1 Regular 2 Regular 3 Regular 4 Regular* 1 Compost 2 Compost 3 Compost

Nitrate Concentration (mg/L) Area S*min Retention Time (min) 1.699 0.09570 8.690 1.328 0.05670 8.701 1.126 0.03550 8.690 2.740 0.2053 8.690 4.800 0.4220 8.674 4.706 0.4121 8.647 4.917 0.4343 8.677 Phosphate Concentration (mg/L) Area S*min Retention Time (min) 0.9134 0.02300 14.010 0.8779 0.02070 14.024 0.8114 0.01640 14.030 1.745 0.07680 14.007 2.539 0.1282 13.977 2.697 0.1384 13.977 2.793 0.1446 13.974

Figure 1. Sample Chromatograph of a Regular soil sample.

Nitrate and Phosphate in Soil Samples Figure 2. Calibration Curve for Nitrate Standards.

Figure 3. Calibration Curve for Phosphate Standards.

Nitrate and Phosphate in Soil Samples Table 2. Statistics for Nitrate and Phosphate content in Regular and Compost Samples.

1 2 3 Average Std. Dev. RSD 95 % CI

1 2 3 Average Std. Dev. RSD 95 % CI

Nitrate Regular (mg Nitrate/g sample) Compost (mg Nitrate/g sample) 0.1669 0.4717 0.1293 0.4582 0.1113 0.4860 0.1358 0.4720 0.02836 0.01394 20.88 2.954 0.06534 to 0.2063 0.4374 to 0.5066 Phosphate Regular (mg Phosphate/g sample) Compost (mg Phosphate/g sample) 0.08709 0.2421 0.08636 0.2653 0.07336 0.2525 0.08227 0.2533 0.007725 0.01163 9.390 4.593 0.06308 to 0.1015 0.2244 to 0.2822

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