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PREPARATION AND USE OF SOIL AND PLANT REFERENCE MATERIALS TO IMPROVE THE QUALITY OF CHEMICAL ANALYSIS AT THE SOILS AND FERTILISERS RESEARCH INSTITUTE (SFRI) Le Thi My Hao, Bui Bich Luong, Bui Hai An,Tran Minh Tien and Paul Milham 1. Reference materials at SFRIt Some reference materials can be purchased but others, e.g. soils and plants, must be prepared in-house. Soil and plant testing for nutrients is a major activity for the Institute and a requirement for the ACIAR project. It is assumed that an accurate result for the reference material indicates an accurate result for the samples analysed side-by-side with them. This process is described as quality control. 2. Collecting the Hanoi soil and plant reference materials The soil: 200 kg of Red River alluvial soil was taken from Bac Ha village, Tho An commune, Dan Phuong district, Hanoi which had been fallowed for more than 10 years. The cabbage: 100 kg of fresh cabbage was collected from the street market outside SFRI. 3. Treatment of the reference materials 3.1. Soils were sieved to remove plant debris and stones. Cabbages had the veins removed. Samples were dried, ground, carefully mixed and divided into two parts. Half of each sample was sent to Australia to become an inter-laboratory proficiency sample. This would provide target values for later use in testing the accuracy of methods and for quality control. 3.2. The remainder was split into containers: 100 containers of soil ~500 g each and 60 containers of cabbage ~50 g each. 3.3. Containers were stored in a chest freezer at -20°C to maintain the integrity. 3.4. The homogeneity of the materials was evaluated by analyzing total N (4 replicates/ container) for all containers. N was chosen as the index because it is poorly distributed in the natural materials. 4. Homogeneity and comparison of the SFRI and ASPAC N measurements The following Kjeldahl N measurements were made by SFRI without knowledge of the Australian values results Parameter SFRI Statistics SFRI/Australia comparisons Comparison with Australian values pHH2O No. Reps 10 8.04 (37) Acceptable Mean 7.96 CV% 0.21 OC (%) No. Reps 20 0.44% (33) Acceptable Mean 0.459 CV% 2.18 Total N (%) No. Reps 20 0.064% (39) Acceptable Mean 0.064 CV% 4.31 Total P2O5 (%) No. Reps 20 P 0.036% (22) P2O5 0.08% Acceptable Mean 0.090 CV% 2.07 Bray-2 P (mg/kg) No. Reps 20 No corresponding data but Bray-1 is 1.4 mg P/kg (8) or 3.2 mg P2O5/kg Acceptable Mean 33.9 CV% 0.49 Available K as K2O (mg/100 g) No. Reps 18 Exch K (cmol/kg) 0.10 (33) 4.7 mg K2O/100 g Acceptable Mean 4.24 CV% 0.95 CEC meq/100 g or cmol/kg No. Reps 20 No corresponding data but Σexcats ~10 cmol/kg (25) No direct comparison The values are in the ballpark Mean 13.2 CV% 1.4 1 0,06 0,061 0,062 0,063 0,064 0,065 N% Soil - Compare N% (mean) 0,066 0,067 0,068 0,069 0,07 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 N% (mean) - ASPAC N% (mean) - SFRI N% Plant - Compare N% (mean) N% (mean) - ASPAC N% (mean) - SFRI 1 2,450 2,500 2,550 2,600 2,650 2,700 2,750 2,800 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 5. Conclusions and future plans 5.1. The homogeneity of the materials reached the target CVs for use as in quality control 5.2. The SFRI and Australian values means are very close showing that the SFRI results are accurate 5.3. During 2016 the reference samples will be used to test the accuracy of the tests for exchangeable soil cations and for Na, K, Ca and Mg in plants 5.4. During 2017 the above procedures will be extended to the micro nutrients Mn, Fe, Zn, Cu, Ni and Mo in plants using AAS. If time permits a colorimetric test for B will be established 5.4. The quality of results for samples will be assured for methods that have been shown to be accurate using side-by-side analysis with the reference samples 5.5. To improve their worth the reference materials will be sent to other labs in MARD and be used to test inter-laboratory performance Comparison of other parameters with ASPAC CV: Coefficient of variation; SFRI: Soils and Fertilizers Research Institute; ASPAC: Australasian Soil and Plant Analysis Council CONTENTS 1. 2. 3. 4. 5. Collecting sample Soil: 200kg Cabbage: 100kg Comparison of the SFRI and Australian values Treatment (sort out extraneous matter, dry, grind and sift through sieve, mix by coning and quartering) Stored in a chest freezer at -20˚C The homogeneity of materials was evaluated by analyzing total N (4 replicates/container) for all containers

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PREPARATION AND USE OF SOIL AND PLANT REFERENCE MATERIALS TO IMPROVE THE QUALITY OF CHEMICAL ANALYSIS AT THE SOILS AND FERTILISERS RESEARCH INSTITUTE (SFRI)Le Thi My Hao, Bui Bich Luong, Bui Hai An,Tran Minh Tien and Paul Milham

1. Reference materials at SFRItSome reference materials can be purchased but others, e.g. soils and plants, must be prepared in-house.Soil and plant testing for nutrients is a major activity for the Institute and a requirement for the ACIAR project. It is assumed that an accurate result for the reference material indicates an accurate result for the samples analysed side-by-side with them. This process is described as quality control.

2. Collecting the Hanoi soil and plant reference materials

The soil: 200 kg of Red River alluvial soil was taken from Bac Ha village, Tho An commune, Dan Phuong district, Hanoi which had been fallowed for more than 10 years.

The cabbage: 100 kg of fresh cabbage was collected from the street market outside SFRI.

3. Treatment of the reference materials3.1. Soils were sieved to remove plant debris and stones. Cabbages had the veins removed. Samples were dried, ground, carefully mixed and divided into two parts. Half of each sample was sent to Australia to become an inter-laboratory proficiency sample. This would provide target values for later use in testing the accuracy of methods and for quality control.

3.2. The remainder was split into containers: 100 containers of soil ~500 g each and 60 containers of cabbage ~50 g each.

3.3. Containers were stored in a chest freezer at -20°C to maintain the integrity.

3.4. The homogeneity of the materials was evaluated by analyzing total N (4 replicates/container) for all containers. N was chosen as the index because it is poorly distributed in the natural materials.

4. Homogeneity and comparison of the SFRI and ASPAC N measurementsThe following Kjeldahl N measurements were made by SFRI without knowledge of the Australian values results

Parameter SFRI Statistics SFRI/Australia comparisons

Comparison with Australian values

pHH2ONo. Reps 10

8.04 (37) AcceptableMean 7.96CV% 0.21

OC (%)No. Reps 20

0.44% (33) AcceptableMean 0.459CV% 2.18

Total N (%)No. Reps 20

0.064% (39) AcceptableMean 0.064CV% 4.31

Total P2O5 (%)No. Reps 20 P 0.036% (22)

P2O5 0.08%AcceptableMean 0.090

CV% 2.07

Bray-2 P (mg/kg)No. Reps 20 No corresponding data but

Bray-1 is 1.4 mg P/kg (8) or 3.2 mg P2O5/kg Acceptable

Mean 33.9CV% 0.49

Available K as K2O (mg/100 g)

No. Reps 18Exch K (cmol/kg) 0.10 (33) 4.7 mg K2O/100 g AcceptableMean 4.24

CV% 0.95

CEC meq/100 g or cmol/kg

No. Reps 20No corresponding data but Σexcats ~10 cmol/kg (25)

No direct comparison The values are in the ballpark

Mean 13.2CV% 1.4

10,06

0,0610,0620,0630,0640,065

N%Soil - Compare N% (mean)

0,0660,0670,0680,069

0,07

2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30

N% (mean) - ASPAC N% (mean) - SFRI

N% Plant - Compare N% (mean)

N% (mean) - ASPAC N% (mean) - SFRI1

2,450

2,500

2,550

2,600

2,650

2,700

2,750

2,800

2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30

5. Conclusions and future plans5.1. The homogeneity of the materials reached the target CVs for use as in quality control

5.2. The SFRI and Australian values means are very close showing that the SFRI results are accurate

5.3. During 2016 the reference samples will be used to test the accuracy of the tests for exchangeable soil cations and for Na, K, Ca and Mg in plants

5.4. During 2017 the above procedures will be extended to the micro nutrients Mn, Fe, Zn, Cu, Ni and Mo in plants using AAS. If time permits a colorimetric test for B will be established

5.4. The quality of results for samples will be assured for methods that have been shown to be accurate using side-by-side analysis with the reference samples

5.5. To improve their worth the reference materials will be sent to other labs in MARD and be used to test inter-laboratory performance

Comparison of other parameters with ASPAC

CV: Coefficient of variation; SFRI: Soils and Fertilizers Research Institute; ASPAC: Australasian Soil and Plant Analysis Council

CONTENTS

1.

2.

3.

4.

5.

Collecting sampleSoil: 200kgCabbage: 100kg

Comparison of the SFRIand Australian values

Treatment (sort out extraneous matter, dry, grind and sift through sieve, mix by coning and quartering)

Stored in a chest freezerat -20˚C

The homogeneity of materialswas evaluated by analyzing totalN (4 replicates/container) forall containers