MS ISO/IEC TR 10037 : 1995
MALAYSIAN
STANDARD
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MS 417 : PART 1 : 1994 ICS : 65.080
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THE ANALYSIS OF FERTILIZERS PART 1 : METHOD OF SAMPLING AND SAMPLE PREPARATION (FIRST REVISION)
STANDARDS & INDUSTRIAL RESEARCH INSTITUTE OF MALAYSIA © Copyright 1
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MALAYSIAN STANDARD MS 417 : Part 1 : 1994 THE ANALYSIS OF FERTILIZERS : PART 1 : METHOD OF SAMPLING AND SAMPLE PREPARATION (FIRST REVISION) The attached amendment on MS 417 : Part 1 : 1994 has been formally approved by the Technical Committee on Fertilizers. Date: 9 May 2001 Amd. 1
(1)
Page 2, subclauses 3.3 and 4.1
To add this NOTE below 3.3 and 4.1:
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NOTE. In the event when the slot cannot be used in a normal sampling of the fertilizer, the sampling has to be done randomly from selected packages according to the scale of sampling as in Table 1. The weight of the sample shall not be less than 250 g.
(2)
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In the event that the fertilizer comes as lumpy material and flakes, where a probe cannot be used then any suitable sampling device may be used. Page 3, Table 2
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Sieve size (mm )
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Type of Fertilizer Ground phosphate rock, compound (ordinary and premium grades), mixtures and organic fertilizers*
2.
Ground magnesium limestone
0.25
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Table 2 on the size requirement of fertilizers for analysis is to be replaced with the following table:
0.50
3. Granular urea, prilled urea, ammonium sulphate, ammonium nitrate, magnesium sulphate, potassium chloride, potassium sulphate, calcium ammonium nitrate, ammonium chloride, diammonium phosphate and single/triple superphosphate
*For total and water-soluble phosphorus analysis only. phosphorus, the sample shall be analysed as received.
MS 417: Part 1: 1994 Amd. 1 Page 1 of 1
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1.00
For citric acid-soluble and ammonium citrate-soluble
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MS 417 : PART 1 : 1994
This Malaysian Standard, which had been approved by the Chemical and Pharmaceutical Industry Standards Committee and endorsed by the Board of the Standards and Industrial Research Institute of Malaysia (SIRIM) was published under the authority of the SIRIM Board in August, 1994. SIRIM wishes to draw attention to the fact that this Malaysian Standard does not purport to include all the necessary provisions of a contract. The Malaysian Standards are subject to periodical review to keep abreast of progress in the industries concerned. Suggestions for improvements will be recorded and in due course brought
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to the notice of the Committees charged with the revision of the standards to which they refer.
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The following references relate to the work on this standard: Committee reference: SIRIM 482/2/2
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Draft for comment: D258 (ISC B)R
Amendments issued since publication Amd. No.
Date of issue
Text affected
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MS 417 : PART 1 : 1994
CONTENTS Page iii
Foreword ..............................................................................................................
iv
1
Scope ....................................................................................................................
1
2
Apparatus ..............................................................................................................
1
3
Sampling of fertilizers in packages ........................................................................
1
4
Sampling of bulk fertilizers .....................................................................................
5
Preparation of sample for analysis .........................................................................
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Tables
Scale of sampling and method of selection ...........................................................
2
Size requirement of fertilizers for analysis .............................................................
2
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Figures
Fertilizer sample probe ..........................................................................................
2
Stream sampling cup .............................................................................................
5
3
Structure of sample riffle ........................................................................................
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Committee representation ...................................................................................
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MS 417 : PART 1 : 1994
Committee representation The Chemical and Pharmaceutical Industry Standards Committee under whose supervision this Malaysian Standard was prepared, comprises representatives from the following Government Ministries, trade, commerce and manufacturer associations and scientific and professional bodies. Federation of Malaysian Manufacturer (Chemical Sector) Malaysian Ceramic Industry Group Malaysian Institute of Chemistry Malaysian Paint Manufacturers Association Ministry of Agriculture (Agriculture Department) Ministry of Defence (Defence, Science and Technology Centre) Ministry of Primary Industries (Geological Survey Department) Ministry of Science, Technology and Environment (Chemistry Department) Petronas (Non-Petroleum Matters)
The Malaysian Society of Soil Science
Dr. Abdul Aziz Hj. Bidin
Malaysian Agricultural Research Development Institute
Dr. Lau Chee Heng
Rubber Research Institute of Malaysia
Dr. Zin Z. Zakaria/Encik Zulkifli b. Hashim
Palm Oil Research Institute of Malaysia
Encik Lee Tat Ping
Malaysian Rubber Producers' Council
Encik Leong Yee Hoe/Encik Peter Shanta
Federation of Malaysia Manufacturers
Encik Leong Cheng Woh
Felda Agricultural Services Corporation
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Encik Poon Yew Chin (Chairman)
Department of Agriculture
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Encik Eddie Chew/Encik Loke Keng Hung/ Encik Wong Kean Hung
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Encik Lee San Chin
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Encik Chan Khoon San
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Cik Fazila Abu Bakar
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The Working Group on Fertilizers which prepared this Malaysian Standard consists of the following representatives:
Cik Mary Ngu Toh Ing (Secretary)
Fertilizer Industry Development Authority Malaysian Industrial Development Authority Malaysian Oil Palm Growers' Council Standards and Industrial Research Institute of Malaysia
Co-opted Members: Dr. Alias Husin/ Dr. Abdul Manaf b. Mohamad Radzi
Petroleum Research & Scientific Services Sdn. Bhd.
Dr. Sharifuddin A. Hamid
National Association Small Holder
Encik Ramakrishnan
FPM Sdn. Bhd.
Encik Hanifuddin b. Abdul Rahman/ Encik Amir Hamzah b. Yasak
Rubber Industry and Smallholder Development Authority
Invited Member: Tuan Hj. Mohd Nor Abu Bakar
ASEAN Bintulu Fertilizers
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MS 417 : PART 1 : 1994
FOREWORD This Malaysian Standard was prepared by the Working Group on Fertilizers with is under the authority of the Chemical and Pharmaceutical Industry Standards Committee. This standard is the first revision of Malaysian Standard MS 417 : Method for the analysis of fertilizers, which was published in 1976. This standard is the first part in a series to provide method of sampling and sample preparation for fertilizers, both in packages and in bulk form. Other parts are as follows:
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2 : Method for the determination of moisture content, particle size and ash content. 3 : Method for the determination of nitrogen. 4 : Method for the determination of phosphorus. 5 : Method for the determination of potassium. 6 : Method for the determination of magnesium. 7 : Method for the determination of boron. 8 : Method for the determination of secondary properties.
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Part Part Part Part Part Part Part
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In this revision, besides giving consideration to local requirement, the following documents have also been referred. Laboratory Manual. General Analytical Laboratory (NFDC-TVA). Tennesse Valley Authority. Division of Chemical Development Fundamental Research Branch. Muscle Shoals, Alabama. April 1979.
(2)
Fertilizer Sampling and Analytical Methods (Fourth Edition). The Fertilizer Institute. Washington, D.C 20036. July, 1982.
(3)
Official Methods of Analysis of the Association of Official Analytical Chemists. 1990.
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(1)
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This revised standard purports to introduce into Malaysia uniform methods of sampling and sample preparation on analysis of fertilizers. It does not deal with the specifications of the materials but prescribes only the method of sampling and sample preparation for fertilizers, both in packages and in bulk form.
This Malaysian Standard supersedes MS 417 : 1976.
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MS 417 : PART 1 : 1994
THE ANALYSIS OF FERTILIZERS PART 1 : METHOD OF SAMPLING AND SAMPLE PREPARATION (FIRST REVISION)
1.
Scope This part of Malaysian Standard prescribes method of sampling and sample preparation for fertilizers, both in packages and in bulk form.
Apparatus
2.1
A non-corrosive (brass, copper or stainless steel) slotted grain probe of sufficient length to penetrate the whole bag diagonally. The probe shall have a continuous slot with sharp edges.
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650 mm (min.)
Length, exclusive of handle 650 mm (min.)
2.1.2
Slot length
2.1.3
Slot width
2.1.4
Inner diameter
2.2
A sample probe and a sample cup as shown in Figure 1 and Figure 2 respectively shall be used.
2.3
Airtight containers which are inert to the material.
3.
Sampling of fertilizers in packages
3.1
In the absence of any other sampling plan agreed upon between the purchasers and suppliers, representative samples shall be obtained in accordance with Table 1.
3.1.1
Lot
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2.1.1
92% of Clause 2.1.1 13 mm
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16 mm
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The dimensions of a typical probe for a 50 kilogrammes bag shall be :
All packages in a single consignment of the material of the same grade and type, drawn from a single batch of manufacture shall constitute a lot. If a consignment is declared to consist of different batches of manufacture, the batches shall be marked separately and the groups of packages in each batch shall constitute separate lots. In the case of a consignment drawn from a continuous process, 2000 packages (or 100 tonnes) of the material shall constitute a lot.
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MS 417 : PART 1 : 1994
3.1.2
The number of packages to be chosen from a lot shall depend on the size of the lot and shall be as given in Table 1. Table 1. Scale of sampling and method of selection Lot size (packages)
Sample size (packages)
1-3 4 - 15 16 - 50 51 - 150 151 - 500 501 - 2000
all 3 10 15 25 35
Method of selection
) ) ) ) )
At random
NOTE. If the lot size exceeds 2000 packages, the sampling cycle is repeated.
The packages selected shall be intact and in good external condition. From each of these packages laid horizontally take a full length diagonal core from bottom corner to top corner or from two opposite corners using the non-corrosive probe. Mix the cores thoroughly to form a representative sample and store in an airtight container.
3.3
When slotting into the bag the slot shall be faced down. When the probe has fully penetrated, turn 180° so that the slot faces upward and is filled before pulling out the probe.
4.
Sampling of bulk fertilizers
4.1
From each lot or batch take 20 samples (cores) at random from different parts and at different depths using a non-corrosive grain probe of 130 cm to 155 cm length. Mix the samples thoroughly and store in an airtight container.
4.2
Taking samples from a moving Conveyor Belt or Chute
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3.2
Take 20 samples (cores) at equal intervals through the whole period of passage of the lot or batch using the sampling cup described in Clause 2.2. Mix the samples thoroughly and store in an airtight container.
5.
Preparation of sample for analysis
5.1
Apparatus
5.1.1
Sample riffle or Reducer
5.1.2
Grinder/Mortar
5.1.3
Balance
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MS 417 : PART 1 : 1994
Procedure
5.2.1
Transfer the collected sample described in Clause 3 and Clause 4 to a suitable sample riffle (see Figure 3). Set the riffle in operation until the sample is reduced to about 250 g.
5.2.2
Grind the sample as rapidly as possible to a fi ne homogeneous powder and the particles should pass through the appropriate sieve size provided in Table 2.
5.2.3
Transfer to a non-corrodible container provided with an airtight closure.
5.2.4
The grounded sample is then sub-sampled for laboratory analysis.
5.3
Precaution
5.3.1
Grinding should be done as rapidly as possible and unnecessary exposure to the atmosphere should be avoided.
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5.2
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E.g. urea is hygroscopic, grinding should be conducted as fast as possible.
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Table 2. Size requirement of fertilizers for analysis
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Ground mineral phosphate e.g. phosphate rock
Sieve size (mm²) 0.25 0.25 0.5 1.0
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Dry powdered fertilizer e.g. ground magnesium limestone
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Granular fertilizers e.g. compound and mixture
Crystalline fertilizer e.g. ammonium sulphate, ammonium nitrate, magnesium sulphate (kieserite)
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Type of fertilizer
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MS 417 : PART 1 : 1994
Figure 1. Fertilizer sample probe
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16 Ga. galvanized iron or 18-20 Ga. Stainless steel, type 304
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Material fabricate from :
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MS 417 : PART 1 : 1994
Figure 2. Stream sampling cup
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MS 417 : PART 1 : 1994
Figure 3. Structure of sample riffle
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MS 417 : PART 1 : 1994
TANDA-TANDA STANDARD SIRIM Tanda-tanda Standard SIRIM seperti yang tertera di bawah adalah tanda-tanda pengesahan dagangan berdaftar. Tanda-tanda ini hanya boleh digunakan oleh mereka yang dilesenkan di bawah skim tanda pengesahan yang dijalankan oleh SIRIM mengikut nombor Standard Malaysia yang berkaitan. Kewujudan tanda-tanda ini pada atau berkaitan dengan sesuatu barangan adalah sebagai jaminan bahawa barangabn tersebut telah dikeluarkan melalui satu sistem penyeliaan, kawalan dan ujian, yang dijalankan semasa pengeluaran. Ini termasuk pemeriksaan berkala kerja-kerja pengeluaran menurut skim tanda pengesahan SIRIM yang dibentuk untuk menentukan bahawa barangan tersebut menepati Standard Malaysia. Keterangan-keterangan lanjut mengenai syarat-syarat lesen boleh didapati dari:
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Ketua Pengarah Institut Standard dan Penyelidikan Perindustrian Malaysia Persiaran Dato’ Menteri, Seksyen 2, Peti Surat 7035 40911 Shah Alam Selangor Darul Ehsan
SIRIM STANDARD MARKS
The SIRIM standard marks shown above are registered certification trade marks. They may be used only by those licensed under the certification marking scheme operated by SIRIM and in conjunction with relevant Malaysian Standard number. The presence of these Marks on or relation to a product is assurance that the goods have been produced under a system of supervision, control and testing, operated during production, and including periodical inspection of the producer’s works in accordance with the certification marking scheme of SIRIM designed to ensure compliance with a Malaysian Standard. Further particulars of the terms of license may be obtained from: Director-General Standards and Industrial Research Institute of Malaysia Persiaran Dato’ Menteri, Section 2. P.O.Box 7035 40911 Shah Alam Selangor Darul Ehsan
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MS 417 : PART 1 : 1994 INSTITUT STANDARD DAN PENYELIDIKAN PERINDUSTRIAN MALAYSIA Institut Standard dan Penyelidikan Perindustrian Malaysia (SIRIM) telah ditubuhkan hasil dari cantuman Institut Piawaian Malaysia (SIM) dengan Institut Negara bagi Penyelidikan Sains dan Perusahaan (NISIR) di bawah Undang-Undang Malaysia Akta 157 pada 16hb. September 1975:Akta Institut Standard dan Penyelidikan Perindustrian Malaysia (Perbadanan) 1975. Institut ini diletakhak dengan kuasa untuk memamju dan menjalankan penyelidikan perindustrian dan untuk menyedia dan memajukan standard-standard bagi baranganbarangan, proses-proses, amalan-amalan dan perkhidmatan-perkhidmatan; dan bagi mengadakan peruntukan bagi perkara-perkara yang bersampingan atau berkaitan dengan maksud-maksud itu. Satu daripada tugas-tugas Institut ini adalah menyediakan Standard-Standard Malaysia dalam bentuk penentuan-penentuan bagi bahan-bahan, keluaran-keluaran, kaedah-kaedah ujian, kod-kod amalan yang sempurna dan selamat, sistem penamaan dan lain-lain. Standard-Standard Malaysia disediakan oleh jawatankuasa-jawatankuasa perwakilan yang menyelaras keupayaan pengilang dan kecekapan pengeluaran dengan kehendak-kehendak yang munasabah dari pengguna. Ia menuju ke arah mencapai kesesuaian bagi maksud, memudahkan pengeluaran dan pengedaran, kebolehsalingtukaran gantian dan pelbagai pilihan yang mencukupi tanpa pembaziran.
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Standard-Standard Malaysia disediakan hanya setelah penyiasatan yang lengkap menujukkan bahawa sesuatu projek itu disahkan sebagai yang dikehendaki dan berpadanan dengan usaha yang terlibat. Hasil ini berasaskan persetujuan sukarela dan memberi pertimbangan kepada kepentingan pengeluar dan pengguna. StandardStandard Malaysia adalah sukarela kecuali is dimestikan oleh badan-badan berkuasa melalui peraturanperaturan, undang-undang persekutuan dan tempatan atau cara-cara lain yang sepertinya.
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STANDARDS AND INDUSTRIAL RESEARCH INSTITUTE OF MALAYSIA
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The Standard and Industrial research Institute of Malaysia (SIRIM) is established with the merger of the Standards Institution of Malaysia (SIM) and the National Institute for Scientific and Industrial Research (NISIR) under the Laws of Malaysia Act 157 on 16th. September 1975: Standards and Industrial Research Institute of Malaysia (Incorporation) Act 1975. The Institute is vested with the power to provide for the promotion and undertaking of industrial research and for the preparation and promotion of standards for commodities, processes, practices and services; and to provide for matters incidental to or connected with those purposes.
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Institut ini beroperasi semata-mata berasaskan tanpa keuntungan. Ia adalah satu badan yang menerima bantuan kewangan dari Kerajaan, kumpulan wang dari bayaran keahlian, hasil dari jualan Standard-Standard dan terbitan-terbitan lain, bayaran-bayaran ujian dan bayaran-bayaran lesen untuk mengguna Tanda Pengesahan SIRIM dan kegiatan-kegiatan lain yang berhubung dengan Penstandardan, Penyelidikan Perindustrian dan Khidmat Perunding.
One of the functions of the Institute is to prepare Malaysian Standards in the form of specifications for materials and products, methods of testing, codes of sound and safe practice, nomenclature, etc. Malaysian Standards are prepared by representative committees which co-ordinate manufacturing capacity and production efficiency with the user’s reasonable needs. They seek to achieve fitness for purpose, simplified production and distribution replacement interchangeability, and adequate variety of choice without wasteful diversify. Malaysian Standards are prepared only after a full enquiry has shown that the project is endorsed as a desirable one and worth the effort involved. The work is based on voluntary agreement, and recognition of the community of interest of producer and consumer. The use of Malaysian Standards is voluntary except in so far as they are made mandatory by statutory authorities by means of regulations, federal and local by-laws or any other similar ways. The Institute operates entirely on a non-profits basis. It is a grant aided body receiving financial aid from the Government, funds from membership subscriptions and proceeds from sales of Standards and other publications, fees and licence fees for the use of SIRIM Certification Mark and other activities associated with Standardization, Industrial Research and Consultancy Services.
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