CALIBRATION OF SOIL NUTRIENT MEASUREMENTS WITH MULTIPLEEXTRACTIONS USING INDUCTIVELY COUPLED PLASMA (ICP)

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Fakultas Pertanian dan Bisnis Universitas Kristen Satya Wacana Jl. Diponegoro 52-60 SALATIGA 50711 - Telp. 0298-321212 ext 354 email:[email protected], website: ejournal.uksw.edu/agric

Terakreditasi Kementrian Riset, Teknologi dan Pendidikan Tinggi berdasarkan SK No 200/M/KPT/2020

Received: 22 April 2022 | Accepted: 7 July 2022

CALIBRATION OF SOIL NUTRIENT MEASUREMENTS WITH MULTIPLE EXTRACTIONS USING INDUCTIVELY COUPLED PLASMA (ICP)

Tia Rostaman, L. Anggria, and A. Kasno

Indonesian Soil Research Institute, Bogor, Jl. Tentara Pelajar No. 12, Cimanggu email: [email protected]

ABSTRACT

Inductively Coupled Plasma (ICP) instrument is a tool used to measure nutrients in the soil, plants, fertilizers, and water, good measurement requires a specific extraction. This study was conducted from March to November 2013 at the Soil Testing and Research Laboratory, Indonesian Soil Research Institute. The soils were collected from the Banten, West Java, and Central Java.

The experiment was carried out by the statistical method of two means. The soil used was 100 g of wind-dried soil, which was analyzed by extracting Morgan Venema, Wet Ashing HNO₃ and HClO₄, Morgan Wolf. The observation was made on the chemical properties of the soil with various concentrations and several extracts. The best extraction was determined based on the value of R² and the significance of the regression equation between the results of soil analysis of several extractions with the percent yield and nutrient uptake as measured by ICP and AAS tools. The experimental results showed that the ICP-OES and AAS tools could be used with some extractions. This was indicated by the significant regression coefficient data on various extraction. The parameters K, Ca, Mg, Fe, Mn, Cu, and Zn were obtained in the HNO₃ and HClO₄ extraction, which could be said to be the best extractions used in ICP and AAS equipment.

Morgan Wolf extract obtained insignificant results on Cu measurements. This showed that the Cu parameters in the Morgan Wolf extract were not suitable for analysis with ICP.

Keywords: ICP, best extraction, critical limit and adequacy limit, macro and micronutrients

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AGRIC Vol. 34, No. 2, Desember 2022: 183-196

INTRODUCTION

The inductively Coupled Plasma (ICP) instrument is a tool used to measure nutrients in soil, plants, fertilizer, and water. To measure properly, a specific extraction is needed to make the tool not damaged, but it is positively correlated with the analysis results. Some extraction can corrode ICP, so it is necessary to study the appropriate extraction. The use of ICP has several advantages, including the ability to identify and quantify all elements except for Argon;

because the sensitivity of the wavelength varies for each determination of an element (Xiandeng Hou et al., 2000). The biggest advantage of utilizing ICP tools when conducting quantitative analysis is the fact that multi-elemental analysis is achievable, and fairly quickly.

Flame Atomic Absorption Spectrometry (FAAS) and Inductive Coupled Plasma- Atomic Emission Spectrometry (ICP-AES) are widely used to determine metallic elements, one of them is cadmium in food products.

Based on research conducted by Nugraha et al. (2012), the low levels of cadmium in most food samples made measurements with FAAS (Shamshad et al., 2009) and ICP-OES (Momen et al., 2006) difficult and required a concentration process; highly sensitive equipment such as Graphite Furnace Atomic Absorption Spectrometry (GF-AAS) (Chwastowska et al., 2004) and Inductive Coupled Plasma-Mass Spectrometry (ICPMS) (Yoshinaga et al., 1999) are required to test trace amounts of cadmium.

To analyze the heavy metal content, ICP MS is used with various considerations, including having the ability to analyze multiple elements

(Arslan et al., 2008) and continue being able to determine more than 60 heavy metal elements with concentrations up to parts per billion (Ashoka et al., 2009), low detection limit (Wuilloud et al., 2004), a detector using a plasma source atomic spectrometry technique (Wuilloud et al., 2004) and a good chromatographic detector (Chiou et al., 2001).

Metal determination usually uses the atomic absorption spectrophotometry method, because this method can be used for the determination of metals in low concentrations (Yunita, 2011). This method is based on the absorption of light by atoms in an excited state. Atomization can be carried out using a flame and without a flame (graphite furnace).

The atomization process with flame has a drawback, namely the amount of analyte that evaporates before atomization occurs and at the time of atomization the resulting atoms can be released into the open air so that the absorption of light by the atoms is getting smaller. The AAS flame detection limit is at the ppm level (10^-6). The weakness of continuous light source AAS cannot be used with absorption lines that are narrower than the band in ordinary spectroscopy. To work around this, a Hollow Cathode lamp is used.

It can only be used for solutions with low concentrations so it requires a relatively large amount of solution (10-15 ml).

Sofyan et al. (2004) mentioned that correlation research is a study to find the best extraction for certain soils and plants. The soil samples used for the experiment are analyzed for their nutrient content to be tested with several extractions. The extraction method is tested on soil conditions with relatively uniform properties or characteristics.

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185 According to Al-Jabri et al. (1987), the

extraction method on soil needs to be tested on soil conditions with relatively uniform properties or characteristics. However, the diversity of soils in Indonesia is quite large and the types of plants cultivated are very varied.

In addition, the absorption of soil nutrients by plants is not the same in all soils, for example, P uptake by corn plants on acid soils is influenced by free Fe₂O₃.

The research on the correlation between test results conducted with ICP with tools and methods that have been tested is AAS.

Furthermore, a correlation experiment is made in the laboratory to find the best extraction using ICP with the extraction selected from the relationship analysis using ICP with the commonly used extraction. The aim of this paper is to determine the critical limit and adequacy limit of each nutrient using the ICP with the best extraction.

MATERIALS AND METHODS

This study was conducted at the Soil Research and Testing Laboratory, Indonesian Soil Research Institute (January - December 2013).

The activity was begun by taking soil samples from several regions in Indonesia with different parent materials and levels of ingredients. The soil samples for this study were taken from several areas in Banten, West Java, and Central Java. The sample selection was based on pH criteria. The soil samples analyzed ranged from 71 samples, the criteria for the pH value (H₂O) of very acidic pH - acid (< 4.5 - 5.5), slightly acidic (5.5 - 6.5), neutral - slightly alkaline (6.6 - 8.5) (Sulaeman et al., 2005). From these criteria, it was hoped that the soil sample could represent soil conditions in Indonesia, especially in Java. The next stage was the

manufacture of several extractions to measure macro and micronutrients using ICP compared to AAS.

This study was carried out using the statistical method of two averages, while the soil used for this study was about 100 g of wind-dried soil and analyzed with various extracts of Morgan Venema, Wet Ashing of HNO₃ and HClO₄, and Morgan Wolf extraction. The observations were made on the chemical properties of the soil with various concentrations and variations of the extraction. The study was conducted with several types of soil that were given extraction, then measured using ICP and AAS. The soil samples used for the experiment were analyzed for their nutrient content to be tested with several extractions. The best extraction was determined by the regression equation between the soil test values of several extractions and the percent yield or nutrient uptake as measured by ICP and AAS. The best extraction was determined by the regression equation which had the highest and most significant r (linear) correlation coefficient.

The calibration of the ICP tool with the AAS comparison was expected to increase the accuracy in the macro-micro nutrients analysis of soil, water, fertilizer, and plants. The correlation between ICP and AAS could be obtained from the correlation curve between the results of macro and micro analysis in various extractors.

RESULTS AND DISCUSSION

The Relationship Between ICP Measurement Analysis Results and AAS Analysis Results in Several Extractions

Figure 1 shows that the relationship between the analysis results of using the ICP and AAS

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tools in the extraction of HNO₃ and HClO₄ have a higher regression value on several macro-micro nutrients compared to other extraction. This is clarified by the regression coefficient data in Table 1, where there are significant differences in the extracts of HNO₃ and HC_lO₄. The wet ashing step is an important step that affects the accuracy of the analysis because ashing can be a source

of uncertainty and contamination from incomplete organic decomposition, volatile matter, and atmospheric contamination (Prihatini, 2010). Wet ashing is one of the preparation steps that can be done to analyze heavy metals. Gonzales (2004) optimized open vessel wet ashing and plant ashing methods for the determination of cadmium, lead, and chromium using ICP-OES.

Graph 1 The regression coefficient graph with extracting HNO₃ and HClO₄using AAS and ICP tools

y = 0,3165x + 13977 R² = 0,1749**

0 20000 40000 60000 80000

0 20000 40000 60000 80000 100000

AnalysisResultsAAS

Analysis Results ICP Fe (mg/kg)

y = 0,779x + 32,822 R² = 0,1429**

200 4060 10080 120

0 20 40 60

Analysis Results AAS

Analysis Results ICP Cu (mg/Kg)

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187 Graph 2 The regression coefficient graph with Morgan Venema extract pH 4.8 using AAS and ICP tools

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Graph 2 shows the relationship between the analysis results of using the ICP and AAS tools in the extraction Morgan Venema pH 4.8. The Mn parameter shows the highest regression value compared to the other parameters. This indicates that the Mn parameter has a significant difference in the Morgan Venema extract pH 4.8. Therefore, it can be concluded that the extraction is measured using either the ICP or AAS, especially the Mn parameter. Soil tests to determine fertilization recommendations have used Multi-Nutrient Soil Analysis (MNS) (Jones and Wolf, 1984), which means that one

type of extraction can be used to analyze more than one nutrient. The MNSA uses a Morgan extract solution of 1 N sodium acetate pH 4.80 with acetic acid. This analysis provides several advantages, including 1) can be used to extract macronutrientsP, K, Ca, Mg, NH₄, NO₃, and SO₄, as well as micronutrients, Cu, Fe, Mn, Zn, and Al; 2) very suitable for soils with a pH range of acid to neutral with a Cation Exchange Capacity (CEC) of 2"35 meq/100 g with a sandy to loamy texture; and 3) suitable for moderately alkaline soils (Jones, 1984).

Graph 3 The Regression Coefficient Graph with Morgan Wolf Extract pH 4.8 using AAS and ICP Tools

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189 Graph 3 shows the relationship between the

analysis results of using the ICP and AAS tools in the Morgan Wolf pH 4.8 extraction. The Fe and Mn parameters show the highest regression values compared to other parameters. This indicates that the Fe and Mn parameters have a significant difference in the Morgan Wolf extract pH 4.8. Therefore, it can be concluded that the extraction is measured using either the ICP or AAS, especially the Mn parameter.

From Table 1, it can be seen that the measurements using the ICP and AAS tools have a significant effect on almost all extractions except for the Cu parameter using the Morgan Wolf extract, which is not significantly different. Moreover, for the other parameters, it looks significantly different. This indicates

that the ICP and AAS can be used in a variety of extractions. The regression coefficients on several extractions indicate that the extraction of HNO₃ and HClO₄that can be said to be the best or recommended for the ICP tool is the extraction of HNO₃ and HClO₄. This is confirmed by the correlation coefficient data reaching 0.95 on parameters K, and Mg. The results of the study show that in measurements using an ICP, it is not recommended to use materials containing salts such as sodium acetate. The use of materials containing salts will make the torch experience simultaneous movement, and it can be seen in the red plasma flame. Thus, this will result in damage to the ICP tool specifically on the torch as the most important part of the ICP tool.

K Regression Equation R²

HNO3+ HClO4

Morgan Venema Morgan Wolf

Y = 1,3942x + 0,0466 Y=1,6659x + 136,67 Y = 1,155x + 111,63

0,95**

0,44**

0,32**

** real at 1% level

* real at 5% level

Ca Regression Equation R²

HNO3+ HClO4

Y = 0,4983x + 0,0024 Y= -7,792x + 10057 Y = -6,3135x + 3532,8

0,47**

0,51**

0,10**

** real at 1% level

* real at 5% level

Mg Regression Equation R²

HNO3+ HClO4

Y = 0,4099x + 0,0274 Y = 0,2178x + 281,22 Y= 0,0977x + 116,1

0,88**

0,62**

0,80**

** real at 1% level

* real at 5% level

Fe Regression Equation R²

HNO3+ HClO4

Y = 0,3165x + 13977 Y = 1,014x + 94,424 Y = 1,0784x–5,0942

0,18**

0,83**

0,98**

* real at 5% level

Mn Regression Equation R²

HNO3+ HClO4

Y = 0,6096x + 318,46 Y = 1,3025x + 19,105 Y = 1,0902x–3,6002

0,75**

0,96**

0,97**

** real at 1% level

* real at 5% level

Cu Regression Equation R²

HNO3+ HClO4

Y = 0,779x + 32,822 Y = -5,9549x + 2,0375 Y = 0,7572x + 1,3233

0,14**

0,18**

0,02

** real at 1% level

* real at 5% level

Zn Regression Equation R²

HNO3+ HClO4

Y = 0,5425x + 56,175 Y = 7,5336x + 2,9813 Y = 4,1372x + 2,6783

0,21**

0,40**

0,76**

** real at 1% level

* real at 5% level

Table 1 The regression coefficient of K, Ca, Mg, Fe, Mn, Cu, and Zn values with several extracts using AAS and ICP

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K Regression Equation R²

HNO3+ HClO4

Y = 1,3942x + 0,0466 Y=1,6659x + 136,67 Y = 1,155x + 111,63

0,95**

0,44**

0,32**

** real at 1% level

* real at 5% level

Ca Regression Equation R²

HNO3+ HClO4

Y = 0,4983x + 0,0024 Y= -7,792x + 10057 Y = -6,3135x + 3532,8

0,47**

0,51**

0,10**

** real at 1% level

* real at 5% level

Mg Regression Equation R²

HNO3+ HClO4

Y = 0,4099x + 0,0274 Y = 0,2178x + 281,22 Y= 0,0977x + 116,1

0,88**

0,62**

0,80**

* real at 5% level

Fe Regression Equation R²

HNO3+ HClO4

Y = 0,3165x + 13977 Y = 1,014x + 94,424 Y = 1,0784x–5,0942

0,18**

0,83**

0,98**

* real at 5% level

Mn Regression Equation R²

HNO3+ HClO4

Y = 0,6096x + 318,46 Y = 1,3025x + 19,105 Y = 1,0902x–3,6002

0,75**

0,96**

0,97**

** real at 1% level

* real at 5% level

Cu Regression Equation R²

HNO3+ HClO4

Y = 0,779x + 32,822 Y = -5,9549x + 2,0375 Y = 0,7572x + 1,3233

0,14**

0,18**

0,02

** real at 1% level

* real at 5% level

Zn Regression Equation R²

HNO3+ HClO4

Y = 0,5425x + 56,175 Y = 7,5336x + 2,9813 Y = 4,1372x + 2,6783

0,21**

0,40**

0,76**

** real at 1% level

* real at 5% level

The Results of Soil Analysis

When taking soil samples, it was based on the soil pH criteria in the field using a Paddy Soils Test Kit (PSTK) and Upland Soil Test Kit (USTK) so that the pH can be seen with the naked eye in the field. The results of the initial soil analysis are presented in Tables 2, 3, and 4.

The soil used for this study varies from acidic to slightly alkaline pH. It is hoped that with these various pHs, various data can be obtained from the nutrient content of the soil.

The method used to measure the cation composition is extraction with Ammonium acetate pH 7.0. The use of the ammonium acetate pH 4.8 method is expected to be analyzed according to the soil pH conditions with very acidic criteria. Ammonium acetate pH 7.0 is a common and widely used method, but this method often gives high analytical results, especially for acid soils.

The soil used for this study has the nutrient content of K, Ca, and Mg, including the medium category. On the micro Fe, Mn, Cu, and Zn, it has a high average content. The

method used in this study with extracts of HNO₃ and HClO₄; Morgan Venema (ammonium acetate pH 4.8) and Morgan Wolf. The use of the morgan Venema method (ammonium acetate pH 4.8) is expected to be analyzed according to soil pH conditions with acid criteria. Meanwhile, the morgan wolf (Sodium acetate pH 4.8) is used to determine the availability of nutrients in the soil. pH 4.8 is intended to approach the pH of the soil around the soil roots. The cations and anions are well soluble in this extraction. The addition of DTPA to the Morgan extraction enhances the ability to extract metals. Morgan Wolf extract is used to determine the availability of macro elements K, Ca, Mg, and micro elements Fe, Mn, Cu, and Zn from the soil.

This extraction is suitable for acidic to almost neutral pH soils

CONCLUSION

Based on the result of this study, the researcher concludes that calibration of soil nutrient measurements shows that the ICP- OES and AAS tools can be used with several extractions. This is indicated by the regression coefficient data, which shows real results in

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191 Table 2 The results of preliminary soil chemical analysis in calibration studies of soil nutrient

measurements at various extractions in the Central Java area

pH(1:5) Organic Ingredients Ammonium Acetate Extract ( CH3COONH4) 1 M pH 7

Sequence H2O KCl C N C/N K Ca Mg Na Total KTK KB

% --- cmol(+)/kg --- %

1 7,47 6,89 1,09 0,04 25 0,30 54,31 4,68 0,61 59,89 66,71 90

2 6,12 5,50 1,46 0,13 11 0,35 23,02 10,49 0,50 34,37 47,83 72

3 5,59 4,94 1,49 0,12 12 0,16 17,06 7,63 0,28 25,12 32,35 78

4 4,87 4,36 2,95 0,21 14 0,08 8,59 2,46 0,22 11,34 20,69 55

5 7,56 7,20 1,32 0,09 15 0,52 30,66 12,69 0,75 44,62 40,36 >100

6 5,89 5,21 1,65 0,14 12 0,20 17,22 7,20 0,30 24,91 29,62 84

7 4,96 4,38 2,91 0,21 14 0,09 7,99 3,18 0,22 11,48 25,90 44

8 5,53 4,83 1,45 0,14 10 0,19 18,39 7,47 0,43 26,47 39,87 66

9 5,63 4,92 2,73 0,20 14 0,27 19,45 7,29 1,19 28,19 30,55 92

10 6,30 5,57 1,77 0,13 14 0,35 35,19 14,75 0,52 50,81 61,75 82

11 7,49 7,01 1,69 0,15 11 0,33 64,92 5,15 0,55 70,96 60,45 >100

12 5,83 5,04 2,10 0,20 11 0,22 38,39 2,49 0,07 41,17 55,11 75

13 5,45 4,94 1,88 0,15 13 0,27 36,56 3,59 0,08 40,52 45,12 90

14 5,59 5,11 3,17 0,19 16 0,19 25,48 6,87 0,77 33,31 35,77 93

15 7,57 6,65 1,91 0,14 14 1,60 30,93 16,22 7,25 55,99 61,50 91

16 5,80 5,11 1,93 0,17 11 0,26 38,88 6,32 0,30 45,77 59,27 77

17 6,78 6,03 1,39 0,09 15 0,39 28,00 8,81 0,87 38,06 33,89 >100

18 5,05 4,49 1,24 0,08 15 0,14 14,48 1,21 0,15 15,97 19,30 83

19 6,64 5,93 2,34 0,11 22 0,40 38,30 13,33 2,22 54,25 63,29 86

20 7,02 6,52 1,26 0,09 15 0,29 55,25 10,52 0,38 66,44 67,03 99

21 7,08 6,18 0,79 0,05 15 0,16 24,77 16,34 0,61 41,88 36,84 >100

22 5,84 5,03 1,68 0,09 18 0,18 24,33 11,56 0,25 36,32 42,52 85

23 5,21 4,57 2,50 0,21 12 0,05 11,22 7,65 0,28 19,20 26,41 73

24 5,22 4,57 2,78 0,25 11 0,11 13,78 8,26 0,41 22,57 30,87 73

25 5,65 5,02 2,00 0,20 10 0,50 15,31 6,47 0,46 22,74 33,47 68

26 5,55 4,73 1,28 0,12 11 0,52 15,40 6,45 0,03 22,40 31,17 72

27 5,74 5,06 1,44 0,10 14 0,26 17,95 6,50 0,37 25,08 31,36 80

28 6,84 6,03 0,64 0,03 18 0,34 10,51 2,62 1,97 15,43 17,41 89

29 5,98 4,74 0,57 0,01 50 0,17 6,93 0,76 2,15 10,00 12,50 80

30 6,26 5,21 0,32 0,02 13 0,30 12,57 4,38 1,52 18,78 21,52 87

31 6,00 5,43 0,85 0,05 19 0,14 8,18 1,44 0,34 10,10 6,85 >100

32 5,36 4,84 0,72 0,03 24 0,09 4,69 0,94 0,27 5,99 3,70 >100

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Table 3 The results of initial soil chemical analysis in calibration studies of soil nutrient measurements at various extractions in the Banten area

Number pH(1:5)

The analysis results are calculated based on a dry soil sample of 105^oC Organic Ingredients Ammonium Acetate Extract ( CH3COONH4) 1 M pH 7

% --- cmol(+)/kg --- %

33 5,37 4,82 1,36 0,12 11 0,18 9,31 2,45 0,13 12,06 9,20 >100

34 5,51 4,90 1,70 0,11 16 0,05 16,02 2,42 0,04 18,53 21,46 86

35 5,83 5,40 2,93 0,21 14 1,42 16,56 2,69 0,01 20,67 23,34 89

36 5,29 4,77 1,30 0,12 11 0,24 7,97 1,55 0,28 10,04 18,33 55

37 5,96 5,31 1,20 0,09 13 0,35 13,91 2,73 0,06 17,05 16,98 100

38 6,18 5,75 1,62 0,10 17 0,29 16,62 2,56 0,05 19,52 17,97 >100

39 6,02 5,39 2,39 0,21 11 0,22 23,16 7,23 0,73 31,34 34,61 91

40 5,63 4,99 2,24 0,18 12 0,56 22,71 9,55 0,51 33,33 38,10 87

41 6,13 5,57 2,29 0,11 21 0,23 25,73 7,48 0,78 34,22 36,89 93

42 5,82 5,19 2,20 0,10 23 0,19 22,63 5,95 0,60 29,36 32,93 89

43 5,54 5,06 2,22 0,18 12 0,19 13,96 6,09 0,52 20,75 24,06 86

44 5,46 5,13 2,02 0,11 19 0,27 16,56 5,55 0,36 22,74 26,59 86

45 4,75 4,24 2,24 0,09 25 0,05 10,40 1,73 0,14 12,32 19,98 62

46 4,39 3,93 2,24 0,10 23 0,14 10,51 1,90 0,14 12,69 20,43 62

47 6,61 6,20 2,04 0,11 19 0,56 29,05 3,18 0,40 33,20 30,73 >100 48 7,41 7,08 1,60 0,09 18 1,29 37,60 3,04 0,15 42,08 24,38 >100 49 5,73 5,04 1,70 0,06 27 0,40 16,74 7,06 0,57 24,77 19,52 >100

Number

pH(1:5)

The analysis results are calculated based on dry soil samples 105^oC Organic Ingredients Ammonium Acetate Extract ( CH3COONH4) 1 M pH 7

% --- cmol(+)/kg --- %

50 5,87 4,80 2,33 0,15 15 0,33 9,54 3,23 0,56 13,66 26,89 51

51 5,15 4,39 2,54 0,15 17 0,64 8,41 3,79 0,73 13,57 27,04 50

52 5,50 4,73 2,22 0,15 15 0,97 8,92 3,85 0,69 14,43 26,60 54

53 5,68 4,96 1,65 0,12 14 0,46 13,94 2,16 0,13 16,68 25,47 65

54 4,96 4,17 2,20 0,14 15 0,64 8,83 3,25 0,59 13,31 30,65 43

55 6,56 6,12 2,16 0,16 14 0,27 25,89 2,42 0,22 28,80 31,76 91

56 6,68 6,22 2,17 0,16 14 0,42 21,09 3,55 0,47 25,53 33,66 76

57 5,57 4,71 2,53 0,18 14 0,71 12,38 4,14 0,80 18,02 31,02 58

58 5,37 4,73 2,18 0,16 14 0,97 15,98 1,81 0,26 19,02 29,19 65

59 5,60 4,77 1,98 0,14 15 0,46 14,66 1,65 0,30 17,07 28,23 60

60 5,30 4,49 3,12 0,23 14 0,41 12,17 2,71 0,64 15,94 31,95 50

61 5,54 4,76 1,92 0,14 14 1,07 13,19 2,99 0,56 17,82 31,44 57

62 5,12 4,49 2,64 0,18 15 0,73 11,11 3,06 0,68 15,58 29,27 53

63 5,13 4,49 3,07 0,20 16 0,53 13,56 2,72 0,67 17,48 30,33 58

64 5,36 4,68 2,41 0,16 15 0,52 13,50 3,65 0,68 18,36 30,23 61

65 4,76 4,03 2,55 0,16 16 0,13 11,20 2,72 0,53 14,59 29,53 49

66 4,99 4,27 1,95 0,09 21 0,34 10,39 1,97 0,46 13,17 22,32 59

67 4,93 4,25 2,16 0,13 17 0,17 10,59 1,72 0,56 13,04 23,29 56

68 5,34 4,52 2,33 0,12 18 0,65 14,07 2,71 0,69 18,12 26,10 69

69 5,40 4,60 2,69 0,14 19 0,79 15,93 3,08 0,61 20,41 28,32 72

70 5,47 4,54 1,49 0,09 17 0,56 14,88 2,47 0,58 18,50 27,27 68

71 5,60 4,80 1,94 0,10 19 0,82 15,28 3,20 0,79 20,09 29,55 68

Table 4 The results of the initial soil chemical analysis in the calibration study of soil nutrient measurements at various extractions in the West Java area

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193 The soil used for this study varies from acidic

to slightly alkaline pH. It is hoped that with these various pHs, various data can be obtained from the nutrient content of the soil. The method used to measure the cation composition is extraction with Ammonium acetate pH 7.0.

The use of the ammonium acetate pH 4.8 method is expected to be analyzed according to the soil pH conditions with very acidic criteria. Ammonium acetate pH 7.0 is a common and widely used method, but this method often gives high analytical results, especially for acid soils.

The soil used for this study has the nutrient content of K, Ca, and Mg, including the medium category. On the micro Fe, Mn, Cu, and Zn, it has a high average content. The method used in this study with extracts of HNO₃ and HClO₄; Morgan Venema (ammonium acetate pH 4.8) and Morgan Wolf. The use of the morgan Venema method (ammonium acetate pH 4.8) is expected to be analyzed according to soil pH conditions with acid criteria. Meanwhile, the morgan wolf (Sodium acetate pH 4.8) is used to determine the availability of nutrients in the soil. pH 4.8 is intended to approach the pH of the soil around the soil roots. The cations and anions are well soluble in this extraction. The addition of DTPA to the Morgan extraction enhances the ability to extract metals. Morgan Wolf extract is used to determine the availability of macro elements K, Ca, Mg, and micro elements Fe, Mn, Cu, and Zn from the soil.

This extraction is suitable for acidic to almost neutral pH soils

CONCLUSION

Based on the result of this study, the researcher concludes that calibration of soil nutrient

measurements shows that the ICP-OES and AAS tools can be used with several extractions.

This is indicated by the regression coefficient data, which shows real results in various extractions. The parameters K, Ca, Mg, Fe, Mn, Cu, and Zn are significantly obtained in the extraction of HNO₃ and HClO₄, while the morgan wolf extract shows no significant difference in the results from the Cu measurement. This indicates that the Cu parameters in the morgan wolf extract show less suitability for analysis on the ICP device.

The extraction of HNO₃ and HClO₄can be said to be the best extraction used in the ICP and AAS as shown by regression data and statistics. The results of the study show that in measurements using an ICP, it is not recommended to use materials containing salts such as sodium acetate. The use of materials containing salts will make the torch experience simultaneous movement, and it can be seen in the red plasma flame.

Thus, this will result in damage to the ICP tool specifically on the torch as the most important part of the ICP tool.

The results of the study show that in measurements using an ICP, it is not recommended to use materials containing salts such as sodium acetate. The use of materials containing salts will make the torch experience simultaneous movement, and it can be seen in the red plasma flame.

Thus, this will result in damage to the ICP tool specifically on the torch as the most important part of the ICP tool.

REFERENCES

A. A. Momen, G. A. Zachariadis, A. N.

Anthemidis, J. A. Stratis. 2006.

Investigation of four digestion procedures

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for multi-element determination of toxic and nutrient elements in legumes by inductively coupled plasma-optical emission spectrometry. Anal. Chim.

Acta. 565: 81-88.

Al-Jabri, M. 2007. Perkembangan Uji Tanah dan Strategi Program Uji Tanah Masa Depan di Indonesia. Hal 54-55 dalam Jurnal Litbang Pertanian, 26(2), 2007.

Arslan, Z & D.H. Secor. 2008. High- Resolution Micromill Sampling for Analysis of Fish Otoliths by ICP-MS:

Effects of Sampling and Specimen Preparation on Trace Element Fingerprints. Marine Environmental Research 66: 364-371.

Ashoka, S., B.M. Peake, G. Bremner, K.J.

Hageman & M.R. Reid. 2009.Comparison of Digestion Methods for ICP-MS Determination of Trace Elements in Fish Tissues. Analytica Chimica Acta 653: 191–199.

B. Q. Shamshad, R. K. Shahidur dan R. C.

Tasrena. 2009. Studies on toxic elements accumulation in shrimp from fish feed used in Bangladesh. As. J.

Food Ag-Ind. 2: 440-444.

Chiou, C.S., S.J. Jiang & K.S.K. Danadurai.

2001. Determination of Mercury Compounds in Fish by Microwave- Assisted Extraction and Liquid Chromatography-Vapor Generation Inductively Coupled Plasma Mass spectrometry. Spectrochimica Acta Part B 56: 1133- 1142.

Gonzales. 2004. Optimization of Open-vessel Wet Digestion and Ashing Methods for Plant materials for Determinant of Cd, Pb, and Cr Using ICP-AES [Thesis].

Malaysia: Universiti Putra Malaysia.

J. Chwastowska, W. Skwara, E. Sterliñska, J.

Dudek, M. Dbrowska dan L. Pszonicki.

2008. GF-AAS Determination of Cadmium, Lead, and Copper in Environmental Materials and Food Products after Separation on Dithizone Sorbent. Chem. Anal. (Warsaw). 53:

887-894

J. Yoshinaga, M. Morita, J. S. Edmonds. 1999.

Determination of copper, zinc, cadmium, and lead in a fish otolith certified reference material by isotope dilution inductively coupled 11 plasma mass spectrometry using off-line solvent extraction. J. Anal. At. Spectrom.14:

1589-1592.

Jones, J.B. Jr., and B. Wolf. 1984. Soil testing procedure using modified (Wolf) Morgan extracting reagent. Benton Laboratories, Inc.Athens, Georgia. 62 p.

Prihatini, R. 2010. Evaluasi Metode Pengabuan Basah Pada Penentuan Timbal dan Kadmium Tanah dengan Kandungan C Organik Berbeda. Hal 1 dalam Skripsi Jurusan Kimia.

Institut Pertanian Bogor.

Sofyan, A., Nurjaya, dan A. Kasno. 2004, Status Hara Tanah Sawah untuk Rekomendasi Pemupukan. Hal 85 dalam Buku Lahan Sawah dan Teknologi Pengelolaannya. Balai Penelitian Tanah, Bogor.

Sulaeman, Suparto dan Eviati, 2009. Petunjuk Teknis Analisa Tanah, Tanaman, Air dan Pupuk. Balai Penelitian Tanah.

Willy Cahya Nugraha, Christine Elishian, Rosi Ketrin. 2012. Penentuan Kadmium Dalam Produk Perikanan Dengan Graphite Furnace Atomic Absorption Spectrometry. Jurnal Kimia Terapan Indonesia. 14(2).

(13)

195 Wuilloud, J.C.A., R.G. Wuilloud, A.P.

Vonderheide & J.A. Caruso. 2004. Gas Chromatography/Plasma Spectrometry an Important Analytical Tool for Elemental Speciation Studies. Spectro- chimica Acta Part B 59: 755-792.

Xiandeng Hou and Bradley T. Jone. 2000.

Inductively Coupled Plasma/Optical Emission Spectrometry in Encyclopedia of Analytical Chemistry R.A. Meyers (Ed.) pp. 9468–9485? John Wiley &

Sons Ltd, Chichester.

Yunita, P. 2011. Penentuan Timah Secara Spektrofotometri Serapan Atom Tungku Grafit. Hal 2 dalam Skripsi Jurusan Kimia. Universitas Andalas, Padang.

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