1、 Collection of SANS standards in electronic format (PDF) 1. Copyright This standard is available to staff members of companies that have subscribed to the complete collection of SANS standards in accordance with a formal copyright agreement. This document may reside on a CENTRAL FILE SERVER or INTRA
2、NET SYSTEM only. Unless specific permission has been granted, this document MAY NOT be sent or given to staff members from other companies or organizations. Doing so would constitute a VIOLATION of SABS copyright rules. 2. Indemnity The South African Bureau of Standards accepts no liability for any
3、damage whatsoever than may result from the use of this material or the information contain therein, irrespective of the cause and quantum thereof. ISBN 978-0-626-22715-9 SANS 1343:2009Edition 3 SOUTH AFRICAN NATIONAL STANDARD Insecticidal solid fumigants that contain aluminium phosphide (food storag
4、e premises) Published by SABS Standards Division 1 Dr Lategan Road Groenkloof Private Bag X191 Pretoria 0001Tel: +27 12 428 7911 Fax: +27 12 344 1568 www.sabs.co.za SABS SANS 1343:2009 Edition 3 Table of changes Change No. Date Scope Foreword This South African standard was approved by National Comm
5、ittee SABS SC 1028B, Pesticides Pesticides efficacy, in accordance with procedures of the SABS Standards Division, in compliance with annex 3 of the WTO/TBT agreement. This document was published in July 2009. This document supersedes SABS 1343:1985 (first revision). A reference is made in 5.5.2(a)
6、and 6.2(f) to product registration with “the relevant government department”. In South Africa, this means the Department of Agriculture (the Fertilizers, Farm Feeds, Agricultural Remedies and Stock Remedies Act, 1947 (Act No. 36 of 1947). A reference is made in 6.1.1 and 6.1.2 to packing in accordan
7、ce with “any other current relevant national legislation”. In South Africa, this means the Hazardous Substances Act, 1973 (Act No. 15 of 1973) and the Fertilizers, Farm Feeds, Agricultural Remedies and Stock Remedies Act, 1947 (Act No. 36 of 1947). Annex A forms an integral part of this standard. An
8、nex B is for information only. SANS 1343:2009 Edition 3 1 Contents Page Foreword 1 Scope 3 2 Normative references 3 3 Definitions 3 4 Requirements 4 5 Test methods. 5 5.1 Aluminium phosphide content and phosphine produced 6 5.2 Ammonium carbamate content . 8 5.3 Paraffin wax content 11 5.4 Ignition
9、properties 13 5.5 Biological efficacy 13 5.6 Behaviour of paraffin wax in sulfuric acid 13 6 Packing and marking. 14 Annex A (normative) Sampling and compliance with this standard 15 Annex B (informative) Quality verification of insecticidal solid fumigants that contain aluminium phosphide . 16 Bibl
10、iography 16 SANS 1343:2009 Edition 3 2 This page is intentionally left blank SANS 1343:2009 Edition 3 3 Insecticidal solid fumigants that contain aluminium phosphide (food storage premises) 1 Scope This standard covers insecticidal solid fumigants that contain aluminium phosphide and are intended fo
11、r use in the fumigation of food storage premises. NOTE Recommendations on the use of aluminium phosphide fumigants are given in SANS 10204. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited a
12、pplies. For undated references, the latest edition of the referenced document (including any amendments) applies. Information on currently valid national and international standards can be obtained from the SABS Standards Division. SANS 5889, Pesticides Biological evaluation of materials containing
13、insecticide(s) having a fumigant action. SANS 10229-1, Transport of dangerous goods Packaging and large packaging for road and rail transport Part 1: Packaging. SANS 10304-1, The classification of pesticides and stock remedies for sale and handling in South Africa Part 1: The classification of pesti
14、cides. 3 Definitions For the purposes of this document, the following definitions apply. 3.1 insecticide chemical substance that is toxic to insects and is used to control infestations of insect pests NOTE Insecticides are derived from substances that occur naturally in plants (for example, pyrethru
15、m) or are synthesized industrially. 3.2 pellet material in the form of an approximately spherical, ovoid, or cylindrical solid with no dimension less than 2 mm SANS 1343:2009 Edition 3 4 3.3 pesticide organic or inorganic substance or mixture of substances used to prevent, destroy, repel or mitigate
16、 pests NOTE Pesticides include insecticides, herbicides, rodenticides, miticides, fungicides, plant regulators and defoliants, and various other substances used to control pests. 3.4 tablets material in the form of pre-formed solids of uniform shape and dimensions, usually circular, with either flat
17、 or convex faces, and of which the distance between faces is less than the diameter 4 Requirements 4.1 Raw materials 4.1.1 General Ingredients of the formulation shall be compatible with one another. 4.1.2 Aluminium powder The aluminium powder used in the manufacture of the formulation shall comply
18、with the following requirements: a) the aluminium oxide (Al2O3) content of the aluminium powder shall not exceed 100 g/kg; b) the iron content of the aluminium powder shall not exceed 1,0 g/kg; c) the total content of lead, copper and zinc of the aluminium powder shall not exceed 0,1 g/kg; and d) th
19、e aluminium powder shall be free of any traces of arsenic. 4.1.3 Ammonium carbamate The ammonium carbamate used in the manufacture of the formulation shall comply with the following requirements: a) the ammonium carbamate content shall be at least 970 g/kg; and b) the dry bulk density of the ammoniu
20、m carbamate shall be 0,725 g/mL 0,005 g/mL. 4.1.4 Paraffin wax The paraffin wax (hard paraffin) used in the manufacture of the formulation shall comply with the following requirements: a) the solidification temperature of the paraffin wax shall be between 58 C and 62 C; b) when the paraffin wax is t
21、ested in accordance with 5.6, colour imparted to the sulfuric acid by the paraffin wax shall not be more intense than that of the reference solution; c) the pH value of the paraffin wax shall be 7 0,2; and d) when determined by any suitable method, the light absorption of the paraffin wax shall not
22、exceed 0,60 at 275 nm, 0,30 at 295 nm and 0,10 above 310 nm. SANS 1343:2009 Edition 3 5 4.1.5 Red phosphorus The iron content of the red phosphorus used in the manufacture of the formulation shall not exceed 0,1 g/kg. 4.2 General requirements for the formulation The formulation shall be in the form
23、of pellets or tablets that are either coated or non-coated with an edible pharmaceutical grade of paraffin (or other water-repellent substance that has a function strictly equivalent to that of the paraffin) and that contain, in addition to the ingredients required for the formulation, a sufficient
24、quantity of ammonium carbamate to suppress the flammability of the formulation. 4.3 Aluminium phosphide content The nominal (stated) aluminium phosphide content of the formulation shall be at least 560 g/kg and the actual content, determined in accordance with 5.1, shall be not less than 560 g/kg an
25、d not more than 585 g/kg. NOTE The aluminium phosphide content is normally 56 % 5 % relative ( 2,8 % absolute) corresponding to about 33 % PH3. 4.4 Phosphine gas produced The quantity of phosphine gas produced by the pellets or tablets, determined in accordance with 5.1, shall be at least 330 g/kg.
26、4.5 Ammonium carbamate content The ammonium carbamate content of the formulation, determined in accordance with 5.2, shall be in the range 260 g/kg to 280 g/kg. 4.6 Paraffin wax content If used, the paraffin wax content of the formulation, determined in accordance with 5.3, shall be at least 29 g/kg
27、. 4.7 Ignition properties When the formulation is tested in accordance with 5.4, no self-ignition shall occur. 4.8 Biological efficacy When the formulation and the reference formulation are tested in accordance with 5.5, the biological efficacy of the formulation shall be at least equivalent to that
28、 of the reference formulation. 5 Test methods NOTE Unless otherwise specified, use only distilled water and reagents of analytical reagent (AR) grade or (when this grade is unobtainable) of the purest grade available. SANS 1343:2009 Edition 3 6 5.1 Aluminium phosphide content and phosphine produced
29、5.1.1 Apparatus 5.1.1.1 Apparatus, as shown in figure 1, and in which the joints between the various glass components are ground-glass joints, not rubber or PVC hoses. 5.1.1.2 Heating mantle, to fit the 100 mL round-bottomed flask. 5.1.1.3 Automatic titrator, with pH meter. Figure 1 Apparatus for th
30、e determination of aluminium phosphide and phosphineSANS 1343:2009 Edition 3 7 5.1.2 Reagents 5.1.2.1 Nitrogen gas, supply of pure nitrogen gas from a cylinder with a regulating valve. 5.1.2.2 Mercuric chloride solution, 15 g of mercuric chloride (HgCl2) dissolved in 1 L of water. 5.1.2.3 Diluted su
31、lfuric acid, 10 % volume fraction solution of concentrated sulfuric acid (d at 25 C = 1,84). 5.1.2.4 Standard sodium hydroxide solution, c (NaOH) = 0,1 mol/L. 5.1.2.5 Methyl orange indicator, 0,5 g/L. 5.1.3 Procedure 5.1.3.1 Transfer 100 mL of the sulfuric acid and 20 drops of the methyl orange indi
32、cator to the first washing bottle, and 100 mL of the mercuric chloride solution to the third washing bottle (i.e. the Friedrichs intensive washing bottle). Leave the second washing bottle empty. 5.1.3.2 Close the stopcocks of the 50 mL dropping funnel and feed a constant flow of nitrogen through the
33、 apparatus at a rate of five bubbles per second. 5.1.3.3 Use a mortar and pestle to finely pulverize five pellets or one tablet, as relevant, of the sample and weigh 50 mg to 80 mg of the powder into a gelatin capsule. NOTE 1 ELI LILLY size No. 1 capsule has been found satisfactory. NOTE 2 The pelle
34、ts or tablet should be crushed speedily to prevent loss of gas by the sample being exposed to the atmosphere. 5.1.3.4 Place the gelatin capsule in the round-bottomed flask and close the flask immediately by inserting the dropping funnel. 5.1.3.5 Flush the apparatus with nitrogen for a further 5 min
35、and then, from the dropping funnel, introduce 25 mL of water and after that 20 mL of the sulfuric acid. 5.1.3.6 Using the heating mantle, heat to just below boiling point and simmer gently for 1,5 h. 5.1.3.7 After completion of the reaction, disconnect the Friedrichs intensive washing bottle and rin
36、se its contents thoroughly and carefully with water into a 400 mL beaker. Rinse the washing bottle at least four times with a total of about 200 mL of water, making sure that no precipitate remains behind. 5.1.3.8 After calibrating the electrode of the pH meter with buffer solutions of pH values 4 a
37、nd 7, determine the pH value of a blank sample consisting of 100 mL of the mercuric chloride solution mixed with only the same quantity of water used in 5.1.3.7 in a 400 mL beaker. 5.1.3.9 Using a magnetic stirrer, titrate the sample solution with the standard sodium hydroxide solution to the same p
38、H value as that observed for the blank sample in 5.1.3.8. 5.1.3.10 Carry out two further determinations as in 5.1.3.1 to 5.1.3.9 (inclusive). 5.1.4 Calculations 5.1.4.1 Calculate the aluminium phosphide (AlP) content, A, of each specimen, expressed in grams per kilogram, as follows: SANS 1343:2009 E
39、dition 3 8 A = 000110334101003457,9611mV= 111,932mVwhere V1is the volume of the standard sodium hydroxide solution used in the titration of the specimen solution, in millilitres; m1is the mass of the sample placed in the gelatin capsule, in grams. Calculate the average of the three results obtained
40、and check for compliance with 4.3 5.1.4.2 Calculate the mass of phosphine (PH3), P, produced from each specimen, expressed in grams per kilogram, as follows: P = 0001103101003411mV= 111,133mVwhere V1is the volume of the standard sodium hydroxide solution used in the titration of the specimen solutio
41、n, in milliltres; m1is the mass of the sample placed in the gelatin capsule, in grams. Calculate the average of the three results obtained and check for compliance with 4.4. 5.2 Ammonium carbamate content 5.2.1 Apparatus 5.2.1.1 Apparatus, as shown in figure 2, comprising a) a heating mantle, to fit
42、 a 500 mL Kjeldahl round-bottomed flask, b) a 500 mL Kjeldahl round-bottomed flask, with ground-glass joint, c) an intermediate part, that connects the flask and the condenser and that has ground-glass joints with teflon collars, and an inlet for the nitrogen. The tube of the inlet reaches almost to
43、 the bottom of the Kjeldahl flask, d) a condenser, with a ground-glass joint, e) an intermediate part, (polyvinyl chloride (PVC) hose), that connects the condenser to a scrubbing tower, and f) a scrubbing tower. SANS 1343:2009 Edition 3 9 5.2.1.2 Gelatin capsules, as in 5.1.3.3. 5.2.1.3 Automatic ti
44、trator, with pH meter. Figure 2 Apparatus for the determination of ammonium carbamate 5.2.2 Reagents 5.2.2.1 Nitrogen gas, supply of pure nitrogen gas from a cylinder with a regulating valve. 5.2.2.2 Sodium hydroxide solution, 50 g/L. 5.2.2.3 Standard hydrochloric acid solution, c (HCl) = 0,1 mol/L.
45、 5.2.2.4 Standard sodium hydroxide solution, c (NaOH) = 0,1 mol/L. SANS 1343:2009 Edition 3 10 5.2.2.5 Mixed indicator Dissolve 0,125 g of methyl red and 0,083 g of methylene blue in 100 mL of ethanol, and filter through a filter paper. NOTE Whatman No. 41 filter paper has been found satisfactory. 5
46、.2.3 Procedure 5.2.3.1 Pour 300 mL of water and 50 mL of the 50 g/L sodium hydroxide solution into the Kjeldahl flask. 5.2.3.2 Pipette 25 mL of the standard hydrochloric acid solution into the scrubbing tower and add 25 drops of the mixed indicator and sufficient water to fill two-thirds of the volu
47、me of the tower. 5.2.3.3 Determine, to the nearest 0,1 mg, the mass of a gelatin capsule. 5.2.3.4 Use a mortar and pestle to pulverize one tablet or five pellets, as relevant, in the shortest possible time, immediately brush into an airtight weighing flask and close the flask. NOTE Owing to the rapi
48、d loss of ammonia gas, the minimum delay is of the utmost importance during the crushing, weighing and transferring of the samples to the apparatus. 5.2.3.5 Fill the tared gelatin capsule with approximately 200 mg of the sample and reweigh the capsule. Calculate the specimen mass in grams. 5.2.3.6 D
49、rop the closed gelatin capsule into the Kjeldahl flask and close the flask by connecting the condenser to it. Begin the nitrogen flow at a rate of five bubbles per second as measured in the tower, and run cold water through the condenser. 5.2.3.7 So regulate the heating mantle that the mixture simmers gently for 2 h. NOTE To avoid loss of the sodium hydroxide solution, the foam level should under no circumstances reach the neck of the condenser. 5.2.3.8 After 2 h, switch off the heating mantle, stop the flow of nitrogen and disconnect the
