Post on 19-Mar-2017
FERTILIZER LABORATORY
Baja- bahan yang ditambah pada tanah untuk menjadikan tumbuhan lebih subur.
Membekalkan nutrien seperti N,K,P,Mg,B dan unsur kimia yang berkaitan dengan proses pembesaran tumbuhan.
PENGENALAN (Analisis baja)
Jenis baja
Baja tunggal* 1 unsur nutrisi dan kadangkala mempunyai ½ unsur kecil lain.
Baja sebatian* Campuran
beberapa baja tunggal yang dicampurkan secara kimia.
Baja campuran* Campuran
beberapa jenis baja tunggal secara fizikal mengunakan
mesin.
Memeriksa unsur-unsur seperti N,P,K,Mg dan B.
Menjaga kualiti produk. Kawalan mutu. Memastikan kandungan nutrisi baja mencukupi
untuk dibekalkan kepada tumbuhan Memeriksa kelembapan baja. Memastikan spesifikasi nutrisi yang dilakukan
oleh pihak kilang dibenarkan oleh RISDA.
Tujuan analisis baja
BAJA
Nitrogen (N)*EA
*Buchi Distillation
Potassium (K)
*Spectrophotometer
*ICP
Magnesium (Mg)*ICP*ASS
Phosporus (P)
*Spectrophotometer
*ICP
Boron (B)*Spectrophot
ometer*ICP
Atomic Absorption Spectroscopy
Flame Photometer
spectrophotometer
Element Analysis
Inductively Coupled Plasma Buchi Distillation
KAEDAH
1. ANALISIS BAJA EA- Elementar Analyzer (Nitrogen shj) Kaedah Kjedahl (manual)2. SAIZ ZARAH (particle size)3. KELEMBAPAN (moisture)4. ICP (Untuk elemen lain kecuali N)
ANALISIS BAJA
KAEDAH PERTAMA(EA-ELEMENTAR ANALYZER)
TIMBANG BAJA
CATAT BERAT (30.000mg)
TAMBAH TUNGSTAN LIPAT TIN KAPSUL
MASUKKAN DALAM TRAY
EA MESIN
KAEDAH KEDUA(KJEDAHL)
TIMBANG (1.00g)
- TABLET KJEDAHL-1/2 SUDU
THIOSULPHATE
ASID TOTAL NSTIRRER
-PANASKAN 180C SELAMA 1 JAM
-NAIKAN SUHU 360C UNTUK 6JAM
-MASUKKAN BORIC ASID
-5 TITIK INDICATOR (N)BUCHI DISTILLATION
TITRATION
SAIZ ZARAH (PARTICLE SIZE)
MASUKKAN DALAM BIKAR
MASUKKAN DALAM
SARINGAN
AYAKLAPISAN 1
LAPISAN 2
LAPISAN 3
MASUKKAN DALAM BIKAR
TIMBANG
MASUKKAN DALAM PLASTIK
KELEMBAPAN (MOISTURE)
ICP (UNTUK ELEMEN LAIN KECUALI N)
Daftar baja
Pindah ke plastik vial
Kisar baja Timbang baja
Isi air 70ml
Isi HCL dan Nitrik Asid
(2:1) Digest
Pindah ke volumetric
flask
Mark up Turas
Pindah ke plastik
vial
-Pindah ke test tube.-ICP
RUMUSAN
NUTRIEN SUMBER KANDUNGAN NUTRIEN (%)
FUNGSI
Nitrogen
Urea
(46% N)
1. Penting dalam pembentukan klorofil dan
kehijauan daun pokok untuk proses fotosintisis.
2. Membantu didalam pembentukan asid amino (protein) dan enzim-enzim yang diperlukan oleh pokok.
3. Membantu pertumbuhan pokok. 4. Meningkatkan berat tandan.
Phosphorus
Rock Phosphate
(32% P2O5)
1. Membantu proses fotosintisis dan proses
pemindahan tenaga.2. Merangsang pertumbuhan akar pokok.3. Penting untuk proses pembiakan.4. Meningkatkan berat tandan.
Potassium
Muriate Of Potash (MOP)
(60% K2O)
1. Membantu didalam proses kimia dalaman
pokok seperti pengeluaran enzim-enzim yang diperlukan oleh pokok.
2. Mengawal keperluan air dan pengangkutan makanan pokok.
3. Menguatkan ketahanan pokok dari penyakit.
Magnesium Oxide
Magnesite Kiesrite
(90% MgO) (27% MgO)
1. Penting dalam proses pembentukan
klorofil. 2. Komponen penting didalam ribosom dan
pembuatan protin.
Boron
Borate
(46% B2O5)
1. Komponen penting didalam proses
penguraian kabohidrat untuk keperluan pokok.
2. Penting untuk pengembangan sel dan tisu pokok.
DATA AKHIR NO. LOKASI JENIS LO DO KILANG JUMLAH ANALISIS NILAI SEPATUTNYA NILAI PERBEZAAN 1=TIDAK MENGIKUT SPESIFIKASI
QTT MAKMAL BAJA KAMPIT % TOTAL % TOTAL % TOTAL MS-MENGIKUT SPESIFIKASI TOTAL BIL STATUS
^N ^P2O5 ^K2O ^MgO ^B2O3 # ^N ^P2O5 ^K2O ^MgO ^B2O3 # ^N ^P2O5 ^K2O ^MgO ^B2O3 # ^N ^P2O5 ^K2O ^MgO ^B2O3 NUTRIEN TMS MS=0,TMS=1
1 1 RISDA 3Z ALL 30 8.9 5.6 17.6 2.0 0.4 34.5 9.0 6.0 18.0 2.0 0.5 35.5 -1.1 -6.7 -2.2 -2.5 -18.0 -2.9 0 0 0 0 0 0 0 0
2 2 RISDA 3Z COSMOS 8.3 5.9 17.2 2.1 0.5 34.0 9.0 6.0 18.0 2.0 0.5 35.5 -7.3 -1.8 -4.4 2.5 -4.0 -4.3 0 0 0 0 0 0 0 0
3 3 RISDA 3Z 8.4 5.7 16.8 2.5 0.5 33.9 9.0 6.0 18.0 2.0 0.5 35.5 -6.2 -5.8 -6.4 25.0 -10.0 -4.6 0 0 0 0 0 0 0 0
4 4 RISDA 3Z 8.5 5.8 16.9 2.6 0.5 34.2 9.0 6.0 18.0 2.0 0.5 35.5 -5.6 -3.7 -6.1 30.0 -8.0 -3.5 0 0 0 0 0 0 0 0
5 5 RISDA 3Z 8.5 5.4 17.2 2.4 0.5 34.0 9.0 6.0 18.0 2.0 0.5 35.5 -5.6 -10.2 -4.4 20.0 -8.0 -4.4 0 0 0 0 0 0 0 0
6 6 RISDA 3Z 8.6 5.5 16.8 2.5 0.4 33.8 9.0 6.0 18.0 2.0 0.5 35.5 -4.4 -8.7 -6.7 25.0 -16.6 -4.8 0 0 0 0 0 0 0 0
7 7 RISDA 3Z 8.5 5.5 17.5 2.6 0.4 34.5 9.0 6.0 18.0 2.0 0.5 35.5 -6.1 -8.0 -2.8 30.0 -12.0 -2.8 0 0 0 0 0 0 0 0
8 8 RISDA 3Z 28 8.4 5.5 17.6 2.4 0.4 34.3 9.0 6.0 18.0 2.0 0.5 35.5 -6.7 -8.8 -2.2 20.0 -12.0 -3.4 0 0 0 0 0 0 0 0
9 9 RISDA 3Z 8.7 5.6 17.2 2.1 0.5 34.1 9.0 6.0 18.0 2.0 0.5 35.5 -3.9 -6.7 -4.4 7.0 -6.0 -4.1 0 0 0 0 0 0 0 0
10 10 RISDA 3Z 8.6 5.6 17.5 2.1 0.5 34.3 9.0 6.0 18.0 2.0 0.5 35.5 -4.4 -6.8 -2.7 7.0 -8.0 -3.4 0 0 0 0 0 0 0 0
11 11 RISDA 3Z 8.4 5.8 17.2 2.1 0.5 34.0 9.0 6.0 18.0 2.0 0.5 35.5 -6.7 -3.3 -4.2 3.0 0.0 -4.2 0 0 0 0 0 0 0 0
12 12 RISDA 3Z 27 8.7 5.4 17.1 2.1 0.5 33.9 9.0 6.0 18.0 2.0 0.5 35.5 -2.9 -10.0 -4.8 7.0 2.0 -4.4 0 0 0 0 0 0 0 0
13 13 LDG. RISDA TG. GENTING RISDA 3Z 8.6 5.5 17.2 2.1 0.5 34.0 9.0 6.0 18.0 2.0 0.5 35.5 -4.4 -9.0 -4.4 7.0 8.0 -4.4 0 0 0 0 0 0 0 0
14 14 E 1 C 1 - 27 ABDFG(7) RISDA 3Z 8.6 5.7 17.3 2.1 0.5 34.1 9.0 6.0 18.0 2.0 0.5 35.5 -4.4 -5.5 -4.2 3.0 -2.2 -4.0 0 0 0 0 0 0 0 0
15 15 RISDA 3Z 8.7 5.5 16.9 2.2 0.4 33.8 9.0 6.0 18.0 2.0 0.5 35.5 -2.9 -7.7 -6.1 12.0 -16.0 -4.7 0 0 0 0 0 0 0 0
16 16 RISDA 3Z 8.6 5.7 17.2 2.0 0.5 34.1 9.0 6.0 18.0 2.0 0.5 35.5 -4.0 -5.3 -4.2 2.0 -1.0 -4.0 0 0 0 0 0 0 0 0
17 17 RISDA 3Z 25 8.6 5.5 17.6 2.1 0.5 34.3 9.0 6.0 18.0 2.0 0.5 35.5 -4.4 -7.9 -2.5 3.0 7.2 -3.5 0 0 0 0 0 0 0 0
18 18 RISDA 3Z 8.5 5.5 17.4 2.0 0.5 33.9 9.0 6.0 18.0 2.0 0.5 35.5 -5.6 -7.8 -3.3 -1.5 -6.6 -4.6 0 0 0 0 0 0 0 0
19 19 RISDA 3Z 8.4 5.5 17.3 2.0 0.5 33.7 9.0 6.0 18.0 2.0 0.5 35.5 -6.2 -9.0 -3.7 0.0 -2.0 -5.0 0 0 0 0 0 0 0 0
20 20 RISDA 3Z 8.6 5.5 17.2 2.2 0.4 34.0 9.0 6.0 18.0 2.0 0.5 35.5 -4.4 -7.7 -4.2 10.0 -12.0 -4.2 0 0 0 0 0 0 0 0
21 21 RISDA 3Z 8.7 5.4 17.4 2.0 0.5 34.0 9.0 6.0 18.0 2.0 0.5 35.5 -3.3 -10.0 -3.1 0.5 -4.0 -4.1 0 0 0 0 0 0 0 0
22 22 RISDA 3Z 8.5 5.5 17.4 2.1 0.5 34.1 9.0 6.0 18.0 2.0 0.5 35.5 -5.1 -8.0 -3.3 4.5 6.0 -4.0 0 0 0 0 0 0 0 0
23 23 RISDA 3S 8.5 5.5 17.5 2.1 0.5 34.0 9.0 6.0 18.0 2.0 0.5 35.5 -5.9 -8.7 -2.8 4.0 -2.0 -4.2 0 0 0 0 0 0 0 0
24 24 RISDA 3S 8.6 5.5 17.0 2.1 0.5 33.8 9.0 6.0 18.0 2.0 0.5 35.5 -4.4 -7.7 -5.3 4.5 5.4 -4.8 0 0 0 0 0 0 0 0
25 25 RISDA 3Z 8.7 5.4 17.1 2.2 0.5 33.9 9.0 6.0 18.0 2.0 0.5 35.5 -3.3 -10.0 -4.8 7.5 -4.0 -4.6 0 0 0 0 0 0 0 0
26 26 RISDA 3Z 8.5 5.8 17.1 2.0 0.5 33.9 9.0 6.0 18.0 2.0 0.5 35.5 -5.6 -3.3 -5.3 2.0 0.0 -4.5 0 0 0 0 0 0 0 0
27 27 RISDA 3Z 8.6 5.5 17.2 2.2 0.5 34.1 9.0 6.0 18.0 2.0 0.5 35.5 -4.0 -7.7 -4.4 12.0 0.0 -3.9 0 0 0 0 0 0 0 0
PURATA 8.6 5.6 17.2 2.2 0.5 34.1 9.0 6.0 18.0 2.0 0.5 35.5 -4.8 -6.9 -4.2 11.1 -6.2 -4.0 0 0 0 0 0 0 0 0
SOLITARY FERTILIZER
* Contain only 1 type of nutrient for plants.
COMPOUND FERTILIZER
* Homogenous, contain 2 or
more essential nutrients. Mixed
through a chemical process.
T Y P E S O F F E R T I L I Z E R
MIXTURE FERTILIZER
* Homogenous, contain 2 or
more essential nutrients.
Doesn't involve chemical process.
EXAMPLE OF FERTILIZER
Urea Kieserite (Kie) Muriate Of Potash (MOP) Ammonia nitrate Ammonia sulphate Ground phosphate rock Baja Organik Espek (BOE) Factory’s fertilizer (K) Risda Fertilizer (RB1, RB2, RB3, RB4)
Main purpos
e
To check the elements ( N,
K, Mg)
Quality
Fertilizer’s
moisture
Enough nutrients for
plant’s growth
To check whether the nutrient’s
specifications that produced by
a factory is correct.
TYPES OF MACHINE USED
Atomic Absorption Spectroscopy
Spectrophotometer
Inductively Coupled Plasma
- Magnesium
-Boron- Potassium- Magnesium- Phosphorus
-Boron- Potassium- Phosphorus
Buchi DistillationElemental Analyzer
- Nitrogen
Flame Photometer
- Nitrogen -The function is same as spectrophotometer
METHODOLOGY
ICP
KJEDAHL
MOISTURE
ELEMENTARY
ANALYSIS (EA)
Back
N
Back
N
Back
MOISTURE CONTENT
Registration Transfer into a plastic vial Grind
Weigh 2.500 g into
a beaker
Pour 70ml distilled waterIsi air
70ml
Pour HCl and Nitric Acid (2:1)
FERTILIZER ANALYSIS: P, K, Mg,B
Heating process (hot plate)
Transfer to the volumetric flask
Mark up the calibration
mark.
Filter the solution Transfer the solution to plastic vial
Transfer to test tube. To be check
using ICP.
FERTILIZER ANALYSIS: P, K, Mg,B
FERTILIZERAim : to determine the contain of element e.g. K, Mg, P, Ca in the fertilizer followed by the specification.
Instrument used:Inductively Coupled Plasma(ICP)- determine all element at one time include heavy metal if necessary.Atomic Absorption Spectrophotometer(AAS) & UV Spectrophotometer - one element at a time.
Determination of pH value
Determination of moisture
content
Determination of potassium
Determination of magnesium
Determination of phosphorus
Trace element
FERTILIZER ANALYSIS
DETERMINATION OF POTASSIUM AND MAGNESIUM
Why we need potassium and magnesium?
POTASSIUM - provide the ionic environment for metabolic process in cytosol.(growth regulation)
- potassium ions (K+) for protein synthesis and opening and closing of stomata.
MAGNESIUM - part of chlorophyll in plant for photosynthesis
METHOD Method for the determination of magnesium
Determination of water-soluble magnesium content (MgO) Principle
Magnesium in magnesium sulphate fertilizers is extracted in boiling water and the magnesium content determined by atomic absorption spectrophotometer.
Reference: MS 417: Part 6: 1994
PROCEDURE•Sample preparation
-registration
-drying
-grinding
•Weigh the sample•Add distilled water and HCl
Digest the solution using hot plate at boiling point around 20minutes
Leave to cool Transfer into volumetric flask and dilute to
the mark (250ml) Mixed the solution and filter in plastic vial
Further dilution(100ml) Add strontium nitrate(5ml) and dilute to the
mark To remove phosphate from magnesium and
calcium and prevent interference from other elements
Preparation for Atomic Absorption Spectrophotometer Standard stock solution
- Potassium dihydrogen sulphate solution- Magnesium sulphate solution
For 1000ppm,weigh 4.3928g. Dry in oven for 2 hours Undergo further dilution(m1v1=m2v2) 0, 0.25, 0.5, 0.75, 1.00 and 1.25 ppm
Pre-calibrate the AAS with standard stock solution
Run the AAS Then, we can determine the concentration
of the solution
DETERMINATION OF PHOSPHORUS
Why phosphorus important to plant?
• Essential to stimulate early plant growth and hastens the maturity.
• Development of root health.• Classified as macronutrient.
Methodology:• molybdovanadate method (yellow method).Reference:•MS 417: Part 4: 1994Apparatus:Spectrophotometer.Principle:•Amount of light transmitted (yellow colour) dependent on the concentration of phosphorus. •Spectophotometric absorption curve from known standard phosphorus solutions determined in unknown solution.
Standard stock solution: Potassium dihydrogen phosphate (4.3928g in 1L) 1000ppm 100ppm (0ppm 2ppm 4ppm 8ppm 10ppm)Reagent used: Molybdovanadate reagent: Ammonium molybdate (100ml)
mixed together with ammonium vanadate (150ml).
Aqua regia: Mixing the HCl & HNO3 together.
PROCEDURE Sample preparation and
weigh the samples (fertilizer)
Add distilled water.
Add 10ml HCl and 5ml HNO3 and boil.
transfer into volumetric flask.
Mark-up with distilled water then filter.
1ml of sample solution is pipette into 100ml volumetric flask.
Add Molybdovanadate reagent and diluted to the mark with distilled water.
prepare calibration standard (0,2,4,6 & 8 ppm) from the stock solution (1000ppm) and take
reading after 30 minutes.
Determine phosphate at acidic colour at pH ± 2.6 Double acid method is used. We put HCl and HNO3 to convert all polyphosphate (P2O7) to
orthophosphate (PO43-).
phosphate + metavanadate = phosphomolybdate acid + water. (yellow colour)
INSTRUMENT: INDUCTIVELY
COUPLED PLASMA (ICP)
INTRODUCTION
INDUCTIVE COUPLED PLASMA (ICP)
measures the light emitted at element-specific characteristic wavelengths from thermally excited analyte ions .
light emitted is separated and measured in a spectrometer, yielding an intensity measurement that can be converted to an elemental concentration by comparison with calibration standards.
Mass spectrometry (MS) 2 type - determination for element having unit PPB-PPT Optical Emission Spectrometry (OES) - determination for element having unit PPM-PPB Gas used: helium and argon Calibration- Manganese Radial – 10PPM axial- 1PPM
PART OF MACHINEAND HOW IT WORK
1. COMPUTER
2. SAMPLER
3. PUMP
4. CHAMBER
5. NEBULIZER
6. FLAME INJECTION
7. TORCH
8. AXIAL / RADIAL
9. SPECTRUM
Selection of colour for each element. Convert into energy Eo Transfer into computer- calculate intensity, log10 = 1/Eo
Can analyze 43 element in the periodic table except for nitrogen and oxygen
Eg: Phosphorus P, Potassium K, Sodium Na, Boron B, Calcium Ca, and etc. Error of ICP : 0.05%
CALCULATION Run standard P, K, Mg, B Plot graph. From graph, calculate slope, m Formula, y=mx + c Calculate intensity Calculate ppm, formulaPPM= (intensity-intercept)/slope