PAS 1160-1988 III ET Standards Association of Australian Standard° '1160—1988 BITUMEN EMULSIONS FOR CONSTRUCTION ANB MAINTENANCE OF PAVEMENTS [Title allocated by Defence Cataloguing Authority: ASPHALT, PETROLEUM (Emulsion, For Pavements) NSC 5610}This Australian Standard was prepared by Committee CH/25, Bitumen and Related Products (for Roadmaking). It was approved on behalf of the Council of the Standards Association of Australia on 20 June 1988 and published on 12 September 1988. The following interests are represented on Committee CH/25: Australian Asphalt Pavement Association Australian Institute of Petroleum Australian Road Research Board Bureau of Steel Manufacturers of Australia Confederation of Australian Industry Institution of Engineers, Australia National Association of Australian State Road Authorities ‘Review of Australian Standards, To keep abreast of roses in indus, Australian Standards or subject Iorpenolc review and are Fep! uptodate bythe Ke of amendments or new edits as necessary Tt 1 Pipa therefore tha Stndeds srs encryption of he et ian any amendments thereto Fulvacats of al SAA publications wil be found inthe Catalogu of SAA Publications; this information [Supplemented each monthby SA's journal ‘The Austral Standard”, which subscribing members {cele and whish pes detels of new publeations, new ediions end amendmens, and of withdrawn Stondande Sigeestions for improvement to Australian Standards, edaresed othe head office ofthe Association, arewecom Nolieaton of any iacewracy ov ambity found tm an Australie Standard shoul Bt ‘ade with dees it Order tha he matte? may be tveigated and appropriate action takenfn AUSTRALIAN STANDARD BITUMEN EMULSIONS FOR CONSTRUCTION AND MAINTENANCE OF PAVEMENTS AS 1160—1988 PUBLISHED BY THE STANDARDS ASSOCIATION OF AUSTRALIA STANDARDS HOUSE, 80, ARTHUR ST, NORTH SYDNEY, N.S ISBN 0 7282 5197AS 11601988, PREFACE This Standard was prepared by the Association’s Committee on Bitumen and Related Products (for Roadmaking) under the direction of the Chemical Standards Board, to supersede AS 1160-1981. This revision incorporates a number of emulsion grades Which were in existence but ‘not encompassed by AS 1160—1981, and also includes new grades which are gradually coming into commercial use. This Standard differs from the 1981 edition in the following ways: (a) Defines @ new class of 67 percent minimum bitumen content emulsion. (b) Allows for bitumen contents of less than 60 percent. (©) Defines new grades of medium setting emulsions, (@) Includes emulsions for short term use. (©) Provides for polymer modified emulsions. (D) Introduces the concept of non-aqueous volatiles (NAV) and the possibility of using @ convection oven to remove water from emulsion in the Residue from Evaporation test. (@) Provides for a sheometer to be used as an alternative to the Engler viscometer. In the light of future experience gained with new grades of emulsion, itis anticipated that further revisions will be made to the specification. Data is currently being collected on transport stability, viscosity measurement, sedimentation and the feasibility of adopting a simple and rapid particle size distribution test method, Users of this Standard who have relevant information are requested to supply this to the Association for consideration by the appropriate committee.1 SCOPE... REFERENCED DOCUMENTS DEFINITIONS .... TYPES AND GRADES ce DESIGNATION ‘COMPOSITION PROPERTIES CONTENTS SAMPLING _ .. TRANSPORT AND STORAGE PURCHASING GUIDELINES MARKING OF DRUMS. APP! m oOMD> “zon co 3 4 5 6 7 8 ‘USE BY’ DATE 9 10 u 2 ENDICES, PURCHASING GUIDELINES SAMPLING .... 7 METHOD FOR DETERMINING PARTICLE CHARGE METHOD FOR DETERMINING RESIDUE FROM EVAPORA- METHOD FOR CALCULATING NON-AQUEOUS VOLA- TILES CONTENT (BY DIFFERENCE) METHOD FOR DETERMINING CONSISTENCY METHOD FOR DETERMINING SIEVE RESIDUE METHOD FOR DETERMINING SEDIMENTATION METHOD FOR DETERMINING STONE COATING ABILITY AND WATER RESISTANCE. METHOD OF DETERMINATION OF BREAKING BEHAVIOUR BY SETTING TIME _... PROCEDURE FOR RECOVERY OF RESIDUE FROM BITU- MEN EMULSION Page ©Copyright — STANDARDS ASSOCIATION OF AUSTRALIA 1988 Users of Standards ace reminded that copyright subsists ia all SAA publications. Except ‘where the Copyright Act otherwise allows, no part ofthis publication may be reproduce, ‘Rored in rerval system in any form or ansntted by any means without prior permission In wrking of the Standards Atgosiation of Australia, Requests (or permission should be directed fo the Head Office of the Association. Where such requests relate to the ‘eproduction of the whole r a substantial part of any Standard, permission may be ondtional on an appropfate royalty payment. AS 1160—1988AS 1160-1988, STANDARDS ASSOCIATION OF AUSTRALIA Australian Standard BITUMEN EMULSIONS FOR CONSTRUCTION AND MAINTENANCE OF PAVEMENTS 1 SCOPE. This Standard specifies requirements for anionic and cationic bitumen emulsions suitable for use in the construction and maintenance of pavements. 2 REFERENCED DOCUMENTS. The following documents are referred to in this Standard. AS 1152 Test sieves 2008 Residual bitumen for pavements 2341 Methods of testing bitumen and related roadmaking products Method 2: Determination of dynamic Viscosity by flow through a capillary tube (AS 2341.2) Method 3: Determination of kinematic Viscosity by flow through a capillary tube (AS 2341.3) Method 4: Determination of dynamic viscosity by rotational viscometer (AS 2341.4) Method 5: Determination of apparent Viscosity by ‘Shell’ sliding plate microviscometer (AS 2341.5) Method 8; Determination of matter insol- uble in toluene (AS 2341.8) Method 9: Determination of water content (Dean and Stark) (AS 2341.9) 3568 Oils for reducing the viscosity of residual bitumen for pavements ASTM D244 Methods of testing emulsified asphalts D146! _ Test method for moisture or volatile distillates in bituminous paving mixtures EI ~ Specification for ASTM thermometers IP Methods for analysis and testing, Part 1, Vot 2, Appendix A BS 2586 Specification for glass and reference electrodes for measurement of pH STPTC Standard methods for testing tar and its products Published by the Standardization of Tar Products Test Commistee 3 DEFINITIONS. For the purpose of this Standard, the following definitions apply Bitumen emulsion—a liquid product in which bitumen is suspended in a finely dispersed state in water by means of emulsifying and stabilizing agents. Anionic emulsion—a type of bitumen emulsion in which the suspended particles are negatively charged. Cationic emulsion—a type of bitumen emulsion in which the suspended particles are positively charged. Oil (cutter oil and flux oil)—hydrocarbon oil derived from the refining of crude oil. (See AS 3568.) 4. TYPES AND GRADES. 4.1 Anionic ype, Grades of anionic emulsion shall be as follows: (@) Rapid-setting (Grade ARS)—an emulsion characterized by rapid breaking and suitable for sealcoat and tackcoat applications but normally unsuitable for mixing with aggregate (b) Medium-setting (Grade AMS)—a general purpose emulsion characterized by an intermediate breaking time and suitable for specialized enrichment, patching and sealing work (6) Slow-setting (Grade ASS)—a general. purpose emulsion with sufficient stability for mixing with water for surface enrichment and for dust laying, and suitable for mixing with soil or. graded aggregates and for use in the grassing of batters and jute meshing. 4.2 Cationic type. Grades of cationic emulsion shall be as follows: (a) Rapid-setting (Grade CRS)—an emulsion characterized by rapid breaking and suitable for sealcoat and tackcoat applications but normally unsuitable for mixing with aggregate, (b) Medium-setting (Grade CMS)—a general purpose emulsion characterized by an intermediate breaking time and suitable for specialized enrichment, patching and sealing work. (c) Slow-setting (Grade CSS)—a general purpose emulsion with sufficient stability for mixing with water for surface enrichment and for dust laying, and suitable for mixing with soil or graded aggregates and for use in the grassing of batters and jute meshing. (@) Aggregate-mixing (Grade CAM)—an emulsion normally used for making cold mix to be stock- piled. 5 DESIGNATION. Designation of the emulsion shall include the emulsion grade as set out in Clause 4, together with the class of bitumen and minimum per- centage of binder in the emulsion. The designations shall be set out as in the examples below. Examples: (@) ASS/170-60 which represents— ASS—anionic slow-setting grade emulsion 170—Class 170 residual bitumen 60—minimum percentage of binder. () CRS/S0-67 which represents— CRS—cationic rapid-serting grade emulsion 50—Class 50 residual bitumen 67—minimum percentage of binder. COPYRIGHT 9 aAS 11601988. “paniigess Bu ede 34 Ins saynoue “ = = PANS] =_ [Ren sy = vine t e 7 = € t c ee Sv 0 Ez SV 10 Ez SV 10 sei.o109 | szroro9 | ses oros | sex orog | sztoro9 | sei orop | set o109 T IbEE S¥ pur 7 xpueddy aa = uus[ ce | wae | wwe | cor woe Tapanddy | siesta duep rh 01 08 "UN, iB . sistastte Aap | oer 09 7 7 = - aa Mpa € t t = t ef ty UNUINEUT “ORES D upuaday a0 sro. sro. 50 0) we 0 SR AT iy TTT “SNST STS ‘puna 2 1 8 o o o or Ge Bun 2 SION 25) a mpuadey co ror| osase|ovsace loose] overse | oxorse (tug sastp een toes =, aM 3 wee wae [wtp ae) ewe TOA TG ae TuBIUOD Ta|AH|GA TOBRDE TON ewe sy ¥ e oF « o o seu Fae 5 RIA aaaay, pu 1 Sion 55 poo % % % # ® o 9p wrasunw “vonsiddena wos} aMpseaL ET Se Bao SSposizap 9509.9}. pur se[8 fuse "wuou clay joussniaejaue | papuose | papsoass | popioass | papioass | papionss | papsoa2s rdsy | "39.0. syon | seer | ager | mon | saan nse Hd ERGE ‘Sauisod | aaiiog | Seve | saIeEN | santo | SnnON aap apnea Spe WV | 2007 SS9 [2PEF SWOPE SUD | SPET Ey | aN GAY | ePUA RIV 19) J0 pours sda aquone 3a soy andorg (ep THON 9a) SOUT (NOISTAWA YAGNIG INIOWAA 09) SALLATOUd NOISTAWA aaa. copyaIGHTAS 11601988 6 COMPOSITION. 6.1 Binder. The binder used in manufacture of emulsion shall be bitumen complying with the requirements of AS 2008, and shall be Class 50, 170 or 320. For special applications the bitumen may be modified with a suitable synthetic or natural polymer. (See Note 3, Table 1.) 6.2 Other ingredients. All other ingredients used in the manufacture of the emulsion shall have no known, deleterious effect on the properties of the residual binder. 7 PROPERTIES. Properties of the emulsion, when determined in accordance with the methods of test prescribed in Tables 1 and 2, shall comply with the Fequirements specified therein for the appropriate grade. 8 “USEBY’ DATE. The emulsion properties shall comply with all the requirements of this Standard up to the ‘use by date. For emulsions listed in Table 1, the ‘use by’ date shall be not less than 90 days from the date of manufacture. For emulsions other than those listed in Table 1 the ‘use by’ date shall be agreed upon between purchaser and supplier. 9 SAMPLING. Sampling shall be carried out in accordance with Appendix B. 10 TRANSPORT AND STORAGE. Emulsions shall be transported and stored in suitable containers. For emulsions transported or stored in bulk, containers may have to be provided with circulation and heating facilities (see Note 1, Table 2). Drums shall be stored away from freezing conditions and shall be rotated end 12 MARKING OF DRUMS. Each drum shall be clearly marked with the following information: (@) Designation of the emulsion in accordance with Clause 5. (b) Manufacturer's name or registered trade mark. (©) Nominal contents. (d) Batch number. (©) Date of manufacture. () The direction, ‘Mix well before use’. (g) ‘Use by’ date, NOTE: Manufacturers who place the number of this Australian Standard on containers, on packaging or on literature related thereto should ensure that the products are manufactured comply with the Standard Attention is particulary drawn to the scheme for independent assurance provided by the StandardsMark which isa registered ‘tification rade mark owned by the Standards Association of ‘Australia and whichis available for use with suitable Australian Standards, ‘The presence of the StandardsMark on or in relation toa product ‘isan assurance that the goods have been produced under «system of supervision, control and testing applied during manufacture and including pesiodieal inspections atthe manufacturer's works in accordance with the ceriieation mark scheme of the SAA ‘The StandardsMark canbe used only by manufacturers licensed Lider the certification mark scheme operated by the SAA, and gnly when accompanied bythe numberof the relevant Avstalian Standard. It will usually be a requirement thatthe wocds Manu factured fo Australian Standard” accompany the number of the Standard and enclose the Mark at shown below: however, ths is'a matter for negotiation with the Assocation Eurther particulars ofthe terms of licence and suitability ofthis Standard for cerineation purposes may be obtained {rom the Quality Assurance and Certifeation Departments Standards Associaion of Australia, 80 Arhur Stree, North Sydney, NSW, ‘over end at intervals of not more than 2 weeks (or as 2060, advised by the supplier). Contents shall be thoroughly mixed before use. The drums should be stored above 40 AUS rp, ground level and where possible under cover. & % s %e 11_ PURCHASING GUIDELINES. Appendix A g 4 contains recommendations and advice on information. 5 2 which should be provided by the purchaser at the time %, & of enquiry or order. % a909 o® TABLE 2 EMULSION PROPERTIES (HIGH BINDER CONTENT) Requirements Gre Nove 1 Manoa of Property CRS grade CAM grade test Viscoiy at 60°C, Pass (ot Note 3), To be recorded To be recorded | AS13413, AS Bai Consintency at 60°C, degrees Enger “To be recorded To be recorded Appendix F (eee Note 3) Residue from evaporation, minimum % by mass @ ‘Appendix D Non-aqueous volatiles content, % by mass] Sax. Gee Nove) “Appendix ‘Sieve residue, maximum $ by mass 025 “Appendix G aril charge ope Positive Appendix C Stone coating ability and water renance, aggregate surace ares coued Appendix 3 Notes: 1, These emulsions have shorter storage life than those in Table 1 and need to be stored and applied at an eleva recommended by the supplier. temperature, as 2 Bitumen emulsions are generally non-newtonian (i. viscosity is shear rate dependant) and because the value measured is an apparent viscority, shear rate should be 3. Method of zest should be in accordance with Appendix F, except thatthe consistency is tested, calculated and reported at 60 £0.2°C instead of 25 +£0.2°C, and two thermometers conforming 10 STPTC Tid, 4. At the discretion of the purchaser, this requirement may be altered, COPYRIGHTAPPENDIX A PURCHASING GUIDELINES (This Appendix does not form an integral part of this Standard) Al GENERAL, Australian Standards are intended to include technical provisions necessary for the supply of material ceferred to in the particular Standard, but do ‘ot purport to comprise all necessary provisions of a contract. In a number of cases the purchaser is either asked to state his requirements, or given a choice of optional requirements. ‘These are contractual matters to be agreed upon between purchaser and supplier. s This Appendix contains detailed explanation, advice and recommendations on information to be supplied by the purchaser at the time of enquiry or order. It aims at avoiding ynisunderstanding of product requirements and should result in the purchaser's receiving satisfactory material and service. A2_ INFORMATION TO BE NOMINATED BY THE PURCHASER. The Purchaser should nominate the following information at the time of enquiry or order after making due reference to the detailed explanation, advice and recommendations contained in this Appendix: (@) Grade of emulsion (Clause 4). (0) Designation indicating bitumen type (Clause 5). (©) Any binder modification required (Clause 6.1). (a) Quantity, with delivery dates and schedulés, and (6) Maximum age at date of despatch. (0) Requirements for consistency if other than those specified (see Note 2 to Table +). (@) Sampling point (see Paragraph BS, “Appendix B), and sampling requirements (see Paragraph B3, Appendix B), (&) Intended use or uses for the emulsion, where appropriate. A3_ INFORMATION TO BE PROVIDED BY THE SUPPLIER. | Where requested by the purchaser at the time of enquiry or order, the following information shall be provided by the supplier: (a) Material safety data sheet. (©) General process of manufacture and packaged types. (©) Any special handling requirements. ry point. coPyAIGHT AS 1160-1988AS 1160-1988 ® APPENDIX B SAMPLING (This Appendix forms an integral part of this Standard) B1 SCOPE. This Appendix sets out methods for the sampling of bitumen emulsion, bitumen (which may be modified with polymer) and oil(s) used in the manufacturing process. B2_ PURPOSE, The purpose of sampling as described in this Appendix is to obtain samples which are truly representative of the material supplied. ‘Samples may be taken for either of the following purposes: (a) To represent, as nearly as practicable, an average of a consignment. (b) To detect any variation within a consignment. B3_ BITUMEN AND OIL. Sampling of bitumen shall be in accordance with AS 2008 and oil in accordance with AS 3568 in any event it shall be appropriate to the consistency and volatility of the material B4 CONTAINERS. Containers for emulsion samples other than rapid setting arades, shall be of 2 L capacity. Screw cap containers or double-tight, friction top cans are suitable, The container shall be thoroughly washed, rinsed with distilled water and dried in an oven. Containers for rapid setting emulsion shall be clean, dry and inert (e.g. glass, plastics or epoxy lined) with tight fitting caps. Containers for bitumen samples shall be clean, dry, 1 L capacity, double-tight, friction top cans. BS PROCEDURE. BS.1 General. The following general considerations apply: (@) Sampling of emulsion may be carried out at the point of loading (.e. at the place of manufacture or depot) or at the point of delivery. (b) Whenever practicable, emulsion should be sampled at the place of manufacture at a time that allows compliance testing to be carried out prior to despatch. (©) Samples may be taken from tanks, drums or other containers used in the storage of transport of the emulsion. (@) Samples of bitumen emulsion containing 60 percent or less bitumen shall be tested as soon as practical after sampling. Samples of high bitumen content emulsion shall either be tested immediately after sampling or be maintained at the storage temperature and tested within the specified storage life of the emulsion. (©) Samples of bitumen emulsion shall be protected from extremes or sudden changes of temperature and from freezing conditions. BS.2 Bulk storage. When sampling is to be carried out from bulk storage, the emulsion shall be mixed thoroughly prior to sampling, the inlet and outlet from the storage tank shall be sealed and three separate samples of at least 2 L shall be drawn from the top, middle and bottom of the tank by one of the following methods: (@) From drain cocks on the side of the tank if these are available and suitably located. Initial emulsion drawn from each cock shall be discarded. (b) By lowering into the emulsion @ weighted can fitted with a stopper (or other suitable tube or thief sampling device as shown in Figure Bl), which may be removed after the can has been lowered to the required depth. (©) By sampling from the circulating spray bar of sprayers during circulation. Each of the three samples may be tested to detect any variation. They shall then be combined and thoroughly mixed to form a composite bulk sample from which a sample shall be drawn immediately for the remaining tests. Alternatively, if the emulsion in the storage tank has been thoroughly mixed and is. homogeneous, a single sample may be drawn from a sampling cock built into a circulating line or located in the discharge line between the tank and suction side of the pump. BS.3 Loading. Sampling during loading shall be carried out as follows: (@) When rail tankers, road tankers, sprayers or drums are being filled, the emulsion shall first be thoroughly mixed and sampling shall be carried out from the COPYRIGHT9 discharge end of the pipelines as the emulsion is flowing through or from the circulating spray bar of sprayers during circulation, A suitable sampling cock in the discharge line may be used to regulate the flow rate into the sampling container(s) (b) The sample shall be collected in three or more increments of about 2 L each at regular intervals during discharge but no portion of the sample shall be taken before the first 10 percent of the consignment has been discharged (©) Approximately 4 L of emulsion shall be withdrawn and discarded before each increment is taken. on (d) The sample increments shall be transferred without delay to a clean, dried bulk container which shall be closed immediately after the addition of each increment, ‘When sampling is completed, the container shall be sealed immediately to prevent loss of volatile material, (©) The bulk sample shall be thoroughly mixed and at least 2 L shall be transferred to asample container allowing 5 percent to 10 percent ullage. The container shall be sealed immediately. : BS.4 Rail and road tankers. Where practicable, the emulsion in the tanker shall be thoroughly circulated or agitated prior to sampling, NOTE: Use of gear pumps may adversely affect the characteristics of the emulsion, Where a sampling cock is available in the delivery line on the tank side of the discharge valve, three separate portions, each of about 2 L, shall be taken, one near the beginning, one near the middle and one near the end of the discharge. In each case, sulficient of the initial material withelrawn shall be discharged to ensure that the sample is representative of the body of the material, In tankers with more than one ‘compartment, each compartment shall be sampled separately. Where a suitable sampling cock is not available, separate samples, each of about 2 L, shall be taken from the top, middle and bottom of the tank by lowering into the ‘emulsion a weighted can fitted with a stopper (or other suitable device, see Figure Bl), which can be removed after the can has been lowered to the required depth. Each of the three incremental samples shall be inspected for evidence of obvious variation, Where any variation exists, incremental samples shall be tested individually. Alternatively, the three samples shall be combined and thoroughly mixed to form a composite bulk sample from which a2 L sample shall be drawn immediately, placed in a clean container and sealed. BS.5. Drums. A number of drums shall be selected at random from each consignment or from each manufactured run, whichever is the smaller. The number ‘of drums selected shall be aot less than the number showa in Table BI. The contents of each drum sclected shall be mixed thoroughly by turning end over end and stirring. As the stirring rod is withdrawn, it shall be examined closely for extraneous matter, unemulsified bitumen or emulsion concentrates produced on standing, From each selected drum a sample of at least 2 L shall be taken out of the centre of the drum by syphoning or by tube thief sampling device (see Figure Bl), Each sample may be tested to detect variations in the emulsion. Where the emulsion is known to be from a single manufactured run, incremental samples shall be combined and thoroughly mixed to form a bulk sample from which a sample of at least 2 L shall be drawn for testing. Where the emulsion is not obviously from a single manufactured run, each batch shall be sampled and tested separately. The volume of each sample shall be at least 2 L. TABLE BI NUMBER OF SAMPLES ‘Number of drums in | Number of incremental armanufactured run ‘samples To 10 ite 30 Sito 100 Ol to 200 201 to $00 Att 700 701 10 1 000 ‘over 1 000, 5 plus | for each $00 drums above 1 000, NOTE: The above proceduce refers 9 nominal 200 L size drums. Wher other sized packages are supplied, Incremental sample volume should be agjusied appropriatly to comply with test requirements COPYRIGHT AS 1160—1988AS 1160—1988 10 BS.6 Test portions. ‘The sample to be tested shall be thoroughly mixed immediately before being subdivided into portions required for individual tests, B6_ SAMPLING PRECAUTIONS. The following sampling precautions shall be ‘observed when sampling: (@) Care shall be taken to prevent contamination of the samples with solvents, cleaning fluids, bituminous materials or other foreign matter. (b) The sample container shall be tightly sealed immediately after the sample is placed in it (©) The sample container shall not be submerged in solvent, nor shall it be wiped with a solvent saturated cloth. Any spilled materials on the outside of the container shall be wiped with a clean, dry cloth immediately after the container is sealed. B7_ SAFETY PRECAUTIONS. Strict precautions shall be taken to avoid injury at all times when handling emulsions. Such precautions include, but are not limited to, the following requirements: (@) Suitable gloves shall be worn while sampling and while sealing containers. (b) Safety glasses or face shields shall be worn while sampling. (©) Smoking shall be prohibited while sampling, (@) Containers should not be held in the hand while sampling hot product. Tongs or some other device shall be used to hold the containers while a hot sample is being taken. (e) The sampler shall stand above and away from the sampling valve or outlet as far as practicable and on the windward side. (©) The sample shall be taken slowly to prevent splashing of the emulsion. (g) The container shall be placed on a firm, level surface to prevent splashing, dropping or spilling of the emulsion during sealing. (h) Local statutory requirements shall be observed. BS LABELLING. Samples shall be securely packed for transport to the testing laboratory and shall be clearly identified by markings on the body and lid of the container. ‘The following particulars shall be shown on the container of label: (a) Designation of the emulsion in accordance with Clause 5. (b) Identification mark. (©) Date of sampling. (4) Where samples are being transported under freezing ambient conditions, such as by air, the containers shall be prominently marked ‘Sample will spoil if frozen; carry ina warm compartment’. (©) Special handling requirements for high bitumen content emulsions. Further information required for identification of the samples shall be supplied on 4 separate sampling form. The additional information shall include the following: (@ Supplier. i) Place and date of sampling. (ii) Quantity of material represented by sample. (iv) Type and identifying number of container or vehicle from which the sample was taken. (%) Name of the sampler. (vi) ‘Use by” date. COPYRIGHTuw AS 11601988 e (9) Tet sampling can (©) Sampling cage in 49 Tight fiting conical cap os Capacity eo 720 mL | _-—False bottom uy Lead weight approx. Tkg (6) Weighted sampling can (@) Bottom-sampling bottle FIGURE 81. EXAMPLES OF SAMPLING DEVICES ‘COPYRIGHT. AS 1e—1988 R APPENDIX C METHOD FOR DETERMINING PARTICLE CHARGE (This Appendix forms an integral part of this Standard) C1 SCOPE. This Appendix sets out a method for determining the nature of the charge on particles of bitumen emulsion, as indicated by the bitumen deposited on electrodes to which an electric current is applied, (C2. PRINCIPLE. Electrodes are immersed in the emulsion. A controlled electric current is applied for a given time and the deposition of bitumen on the electrodes is observed. C3 APPARATUS. The following apparaius is required: (@) Variable direct current voltage source. A variable direct current voltage source of about 12 V capable of supplying at least 8 mA during the test, and an ammeter. A suitable circuit for such equipment is shown in Figure Cl (b) Electrodes, Electrodes consisting of two stainless stee! plates approximately 75 mm long and about 25 mm wide with an immersion mark at 25 +2 mm. An insulating device is used to hold the plates parallel 25 2 mm apart in the emulsion sample during the test. (©) Glass beaker. A glass beaker of 150 mL or 250 mL capacity, (@) Timing device. A timing device graduated in at least 1 min intervals. C4 PROCEDURE. The procedure shall be a follows: (a) Suspend the electrode assembly in the beaker. (b) Pour the emulsion into the beaker uni the electrodes are immersed toa depth of 25 mm. (©) Connect the leads from the electrodes to the current source through the milliammeter and variable resistor. (@ Adjust the current to about 8 mA and start the timing device. (©) When the current reading has dropped to about 2 mA, or at the end of 30 min, whichever occurs first, disconnect the current source and gently wash electrodes in running water. (0) Observe electrodes for bitumen deposition. CS REPORT. Results shall be reported as follows: (@) If an appreciable layer of bitumen is deposited on the anode, report particle charge as negative. (b) If an appreciable layer of bitumen is deposited on the cathode, report particle charge as positive. 2 Ge suppiy 3 176 wohage FIGURE C1. CIRCUIT FOR VOLTAGE SOURCE COPYRIGHT8 “As 1160-1988 APPENDIX D. METHOD FOR DETERMINING RESIDUE FROM EVAPORATION (This Appendix forms an integral part of this Standard) D1 SCOPE. This Appendix sets out a method for determining the residue from evaporation of bitumen emulsion. D2_ PRINCIPLE. A sample of the emulsion is weighed into a container, evaporated ‘ona hotplate to remove water and reveighed. Residue from evaporation is calculated from the mass of the sample and residue after evaporation. D3_ APPARATUS. The following apparatus is required: (a) Hotplate. A hotplate with variable temperature control. (©) Thermostaticaly controlled cunve-tion oven. A thermostatically controlled convection oven capable of maintaining a temperature within the range 105°C to 110°C. (©) Metal or glass container. A metal or glass container approximately 75 mm in diameter and 105 mm deep, provided with a small wire or glass stirrer. (a) Desiccator. (©) Balance. A balance of suitable capacity, accurate to 0,003 g and readable to 0.001 g, D4 PROCEDURE. The procedure shall be as follows: (@) Dry the container in a thermostatically controlled convection oven at 105°C to 110°C for I'h and allow it to cool in a desiccator. (b) Tare the coniainer and stirrer. (©) Weigh 10 +1 g of the emulsion into the container; record the mass of the sample to the nearest 0.001 g (rn). (@) Place container on hotplate and heat at rate just sufficient to evaporate water without undue frothing. Continuously stir the emulsion to break any bubbles AS soon as the water has been driven off (indicated by cessation of bubbling followed by the appearance of incipient white fumes), remove the container from the hotplate and allow to cool in the desiccator. NOTE: Alternatively, a forced draft ventilated oven may be used to remove water from the emulsion Provided that this method is calibrated agaist the hotplate method for water removal (©) When cool, remove from desiccator, accurately reweigh container and stirrer, and determine the mass of the residue (7m:) to the nearest 0.001 8, D5_ CALCULATION AND EXPRESSION OF RESULT. Calculate the residue from evaporation as a percentage by mass of the emulsion as follows: Residue, percent = 7% x 100 mass of residue mass of sample, where m: mm, D6 REPORT. Report the residue from evaporation to the nearest 0.1 percent. ‘COPYRIGHTAS 11601988 APPENDIX E METHOD FOR CALCULATING NON-AQUEOUS VOLATILES CONTENT (BY DIFFERENCE) (This Appendix forms an integral part of this Standard) E1_ SCOPE. This Appendix sets out a method for calculating the non-aqueous volatiles content (NAV) of bitumen emulsion. Where a flux oil has been incorporated in the emulsion, the non-aqueous volatiles content may be determined by distillation as described in’ ASTM D1461. E2_ CALCULATION AND EXPRESSION OF RESULTS. Calculate NAV as follows: NAY, percent by mass = 100 - (C + W) where c Ww residue from evaporation (as determined in Appendix D) ‘water content (as determined in accordance with AS 2341.9). E3_ REPORT. Report NAV to the nearest 0.1 percent. coPyaiGHT1s APPENDIX F METHOD FOR DETERMINING CONSISTENCY (This Appendix forms an integral part of this Standard) F1 SCOPE. This Appendix sets out a method for determining consistency of bitumen emulsion in arbitrary units at 25°C using the Engler viscometer. F2 PRINCIPLE. The efflux time of an emulsion at 25°C from an Engler viscometer is compared with that for water at the same temperature and from the same instrument. The ratio of the times obtained is expressed as degrees Engler. F3 APPARATUS. The following apparatus is required: (a) Engler viscometer. Engler viscometer consisting of a cup with a short jet in the ceritre of the base which is stoppered by means of a tapered, hardwood plug. ‘The cup is surrounded by a waterbath fitted with a stirring device (see Figure Fl). (b) Volumetric receiving flask. A volumetric receiving flask of 200 mL capacity at ; 20°C. (©) Two thermometers. Two thermometers complying with Specification IP76C or two standard thermometers complying with No 23C of ASTM Designation El (@) Sieve. A sieve having an aperture size of 600 um complying with AS 1152. (©) Timing device. A timing device of any suitable type which can be read to 0.2 s or less, and is accurate to 0.07 percent when tested over $ min. F4_ VERIFICATION OF THE VISCOMETER. The procedure for verification of the viscometer shall be as follows: (@) Wash the cup with a jet of xylene, then several times with alcohol and finally with distilled water. (©) Set up and level the viscometer so that the measuring and levelling projections are in the same horizontal plane. (©) Insert a stopper which has been used only for the water test of the apparatus and has never been in contact with oil or emulsion, (d) Fill the volumetric receiving flask nearly to the brim with distilled water at 20°C and pour into the viscometer cup and allow the flask to drain in an inverted position for 3 min, (©) Fill cup to a little above the pointers. (® Place lid and thermometers in position and maintain temperature of water in the cup and bath at 20 £0.5°C. (a) Raise stopper a few times to fill jet completely with water and wet surface of the outlet so that a drop completely covering the surface remains hanging, (h)_ Set water surface exactly at the pointers by sucking out excess water with a pipette or, if necessary, by adding a small quantity of water at 20°C. () When water is completely at rest, place drained receiving flask underneath the orifice. Lift stopper right out vertically so that the surface of water suffers minimum disturbance and at the same time start timer. (&) Note the time taken for receiving flask to fill to the 200 mL mark. (1) Repeat determination until three consecutive results have been obtained differing by no more than 0.5 s. Clean apparatus and make another series of determinations in the same way. If agreement is obtained with the results of the first series, no further tests need be made; if not, carry out further series of determinations until constant times of efflux are found. (n) The mean of the six values of the last two series is taken as the time of efflux of water and shall lie between the limits of 47 5 and 53 s NOTE: If the rime of efflux of water les outside these limits, the orifice should be replaced, or ‘viscometer which conforms 10 the requied limits should be used. Verification procedure required to be carried out at regular intervals (m) FS DETERMINATION OF THE FACTOR FOR THE VISCOMETER. Repeat procedure described in Paragraph F4 at 25 +0.2°C, calculate the mean of values Obtained and record as the factor for the viscometer (Ty). COPYRIGHT AS 11601988AS 1160-1988 6 F6 PROCEDURE. The procedure shall be as follows: (a) Wash cup as described in Paragraph F4(a) and dry. (b) Adjust temperature of water in the jacket of the viscometer to 25 +0.2°C and insert stopper in the cleaned cup. (© Pour emulsion through the 600 um sieve into the viscometer cup until the level of the surface makes contact with one or more of the pointers and adjust levelling screws, if necessary. Add more emulsion until the surface of the emulsion makes contact with all three pointers simultaneously. (@)_ Remove excess emulsion with a pipette; do not draw any off by raising the stopper because coagulation of bitumen may occur in the jet when stopper is reinserted. (©) When the temperature of jacket and emulsion is steady at 25 +0.2°C, measure time of efflux of 200 mL of emulsion into receiving flask allowing emulsion to flow down the side of the flask to prevent frothing. Where frothing obscures the meniscus, the test shall be repeated from Step (a) above. NOTE: Measurement shouldbe caried out a son as possible after fling viscometer ensuring that Temperature of emulsion is maintained at 28 202°C (8) Carzy out three determinations om three separate portions of the sample and take the mean value (7.). If any of the three determinations differ by more than 5 percent of the mean value, carry out three further determinations. (®) After each determination, wash out the cup with distilled water and remove ‘superfluous water with filter paper. Clean jet with a folded piece of filter paper ‘or pipe cleaner moistened with xylene and dry the base of the instrument round the jet with filter paper. F7_ CALCULATION AND EXPRESSION OF RESULTS. Calculate consistency in degrees Engler at 25°C as follows: q 7 Consistency at 25°C mean efflux time of emulsion efflux time of water. F8 REPORT. Report consistency to the nearest 0.1 degrees Engler at 25°C. 306 +1 | 20 + 0.142.804 0.024. 5 40.2] DIMENSIONS IN MILLIMETRES. FIGURE F1. ENGLER VISCOMETER COPYRIGHT” APPENDIX G. METHOD FOR DETERMINING SIEVE RESIDUE (This Appendix forms an integral part of this Standard) G1 SCOPE. This Appendix sets out a method for determining the quantity of bitumen emuision residue which is retained on a specified sieve. G2 APPARATUS. The following apparatus is required: . (a) Sieve. A sieve complying with AS 1152, fitted with a wire mesh having an. aperture of 150 ym in a frame of about 75 mm diameter and about 25 mm depth. (b) Balance. A balance of at least 200 g capacity, accurate to 0,003 g and readable to 0.001 g. (©) Glass conical flask or becker, A glass conical flask or beaker of 250 mL capacity. (a) Glass beaker. A glass beaker of 600 mL capacity. (©) Watch glass. A watch glass of about 100 mm diameter. (© Thermostatically controlled oven. A thermostatically controlled oven with ventilation, capable of maintaining a temperature within the range 105°C to 110°C. (g) Solution of surfactant. A solution of surfactant compatible with the emulsion. + NOTE: If available from the supplier, the surfactant solution should be used, If such a medium is ‘ot supplied, then for cationic emulsion, a solution (say Z percent in wate) of a eatonie surfactant ‘may oe empioyed, and for anionic emulsion, any suxable anionic surfactant may be employed G3 PROCEDURE. The procedure shall be as follows: (a) Weigh approximately 100 g of sample to the nearest 0.1 g (m,) into the 250 mL. conical flask or beaker. (b) Wash, dry and weigh the sieve together with the watch glass to the nearest 0.001 (mn). (©) Place the sieve over the 600 mL beaker and wet it with the surfactant solution. Pour the emulsion rapidly through the sieve and rinse the 250 mL. flask or beaker with the surfactant solution to remove any remaining emulsion and pour over the sieve! (@) Rinse the sieve and its contents with the surfactant solution, followed by distilled water. Examine the sieve for any retained material, Place the sieve on the watch glass and dry the sieve, watch glass, and residue in the oven at 105°C to 110°C. for 1 h and weigh to the nearest 0.001 g (ms). G4 CALCULATION AND EXPRESSION OF RESULTS. Calculate sieve residue as a percentage by mass of the emulsion as follows: Sieve'residue, percent by mass = x 100 where m: im, ms mass of sample mass of sieve with watch glass mass of sieve, watch glass and residue. G5 REPORT. Report sieve residue to the nearest 0.01 percent. ‘COPYRIGHT AS 1160-1988AS 1160-1988 APPENDIX H METHOD FOR DETERMINING SEDIMENTATION (This Appendix forms an integral part of this Standard) H1_ SCOPE. This Appendix sets out a method for determining the degree of sedimentation of bitumen emulsion on standing undisturbed. It provides a means of evaluating the tendency for the two phases of emulsion to separate with time. H2 PRINCIPLE. The emulsion is allowed to stand for three days, after which the water content is determined on the top and bottom layers and the difference is calculated and taken as a measure of sedimentation. H3_ DEFINITION. ‘Sedimentation—settling of the particles of an emulsion due to the action of gravity, This phenomenon must not be confused with the separation of the disperse phase due to instability of the emulsion (coagulation), Hé APPARATUS. The following apparatus is required: Two glass-stoppered measuring cylinders. Two 500 mL_glass-stoppered measuring cylinders, SO S$ mm outside diameter graduated at each $ mL. NOTE: The measuring cylinders may be fitted with wo glass stopcocks at graduations $0 mL and 450 mL. The stopeocks, where fited, should have a minimum bore of # nim HS PROCEDURE. The procedure shall be as follows: (@) Stir the sample of emulsion until thoroughly mixed and pour $00 mL into each of the two glass measuring cylinders. () Stopper the cylinders and allow them to stand undisturbed at laboratory temperature for three days. (©) Remove from each cylinder, approximately the top 50 mL of the emulsion without disturbing the remainder of the emulsion, by opening the top stopcock or by withdrawing the emulsion carefully by pipette or siphon. (d) Place each portion in a separate beaker, stir thoroughly with a stirring rod and determine water content in accordance with AS 2341.9. (©) From the remainder of the test portion, remove and discard the next 400 mL. of emulsion from each cylinder by opening the bottom stopcock or carefully by means of a pipette or siphon. (0) Thoroughly stir the emulsion remaining in each of the two cylinders and determine the respective water contents in accordance with AS 2341.9. H6 CALCULATION AND EXPRESSION OF RESULTS. Calculate sedimentation of the sample as follows: Sedimentation, percent, by mass = B - A where B A H7 REPORT. Report sedimentation as a percentage to the nearest 0.1 percent. average of the percentage of water from the two top layer portions average of the percentage of water from the two bottom layer portions. coPyRIGHT19 APPENDIX J METHOD FOR DETERMINING STONE COATING ABILITY AND WATER RESISTANCE (This Appendix forms an integral part of this Standard) J1_ SCOPE, This Appendix sets out a metiiod for estimating if bitumen emulsion ‘can coat an’ aggregate uniformly and thoroughly. It also provides a method of estimation of how well the coating can withstand the stripping effect of water. 32 APPLICATION. This method is applicable to both dry and damp aggregates and provides a means of evaluating a cationic emulsion for plant mix work, either for immediate laying or for stockpiling. 43 PRINCIPLE, The emulsion is mixed in a prescribed manner with a standard aggregate mixture which is then visually examined for coating. Two ‘indicator’ aggregates are used since their light colour facilitates stone coating assessment. After a curing period, the coated aggregate is sprayed with water and visually examined - to assess the total proportion of surface area covered with binder. J4 MATERIALS. Three types of crushed aggregates are required as specified elow. Each ageregate shall be sieved to pass a 9.5 mm aperture size sieve complying with AS 1152 and be retained on a 4.75 mm aperture size sieve complying with AS 1152, and shall be washed and dried) ss 500 g batches shall be prepared as follows: 400 g dolerite from Prospect quarry, N.S.W.* 50 g white quartz (indicator) from Tenterfield, N.S.W.* 50 g limestone (indicator) from Cow's Flat, N.S.W.* JS APPARATUS. The following apparatus is required: (a) Porcelain evaporating dish. Porcelain evaporating dish about 230 mm diameter (b) Non-metaitic spatula, A non-metallic spatula with a blade approximately 19 mm wide, rounded at both ends. (©) Balance. A balance of at least 2 ke capacity accurate to 0.3 g and readable to O1g. (a) Stopwatch or clock. A stopwatch or clock with seconds display, (©) Water spraying apparatus. A water spraying apparatus for applying tap water in a low-velocity spray under a constant head of 900 +75 mm, through a 19 mm tube and a 100 mm diameter spray nozzle with holes approximately 1.5 mm diameter and evenly spaced at about 9 mm centres. (O Glass'beaker. A glass beaker of 100 mL capacity with lip and glass stirring rod. 46 TEST CONDITIONS. The test shall be carried out in a test room or compartment free from strong draughts, maintained at a temperature of 23 +2°C, JT PROCEDURE. The procedure shall be as follows: (a) Allow apparatus and materials to equilibrate with the test conditions. (b) Place a 500 g charge of test aggregate into the porcelain dish and spread flat (©) Stir the sample of emulsion until thoroughly mixed and weigh into a 100 mL beaker sufficient of the sample so that 35 +2 g will be delivered on pouring, (@ Pour 35 +2 g of emulsion as uniformly as possible over the test aggregate and without delay start the stopwatch and commence mixing in the following manner: (i) Turn the aggregates in from the edge to the centre at about two strokes of the spatula per second. (i) For each stroke, push the spatula lengthwise into the aggregates in the dish to the full depth of the material and at an angle of about 30 degrees to the horizontal. (iii) Cast the material towards the centre of the dish on each stroke by lifting and rotating the spatula. * Stocks of these agaregates are availabe from the Engineer-Manager, Central Asphalt Depot, Department of Main Roads, Granville, NSW, COPYRIGHT AS 1160—1988AS 11601988 2» (iv) Between each stroke rotate the dish about 45 degrees in a constant direction. (©) Continue mixing for 180 25 s and drain off excess emulsion by tilting the dish for several minutes. (®, Remove approximately one fifth of the mixture, place it on absorbent paper and evaluate the coating as satisfactory or not. Coating is classed as satisfactory if all stones are completely coated with emulsion (substantially unbroken at this stage) which is not ‘thin’ or ‘watery’, and no white stone is showing through. (g) Set aside remainder of the mixture for 30 minutes without further disturbance. (b) Spray mixture gently with tap water of hardness less than 250 parts per million calcium carbonate (CaCO) until inundated, then carefully decant. Continue ‘treatment until the overflow water runs clear. Drain off remaining water in the dish and transfer mixture onto absorbent paper with the minimum of disturbance. (Repeat Steps (b) to (h) above using aggregate dampened with 1.5 to 2.0 percent water. J8 EVALUATION. Evaluate the coating visually to estimate the total percentage aggregate surface area that is coated with binder. The deposited film of binder is only acceptable if it is of sufficient thickness to obscure the colour of the aggregate or if it is sticky to the touch. A darkish stain is not to be construed as binder coating, Repeat evaluation after the mixture has been air dried. A fan may be used to air dry the mixture if desired. 439 REPORT. The following information shall be reported for both dry and damp ratings: (a) Condition of the aggregate initially, viz ‘dry’ or ‘damp’, (b) Coating properties of the emulsion as described in Paragraph J7(f). (©) Resistance of the deposited film of binder to stripping by water, as the ‘percentage of aggregate surface area coated’, according to the higher of the two assessments in Paragraph J8. ‘COPYRIGHTa APPENDIX K METHOD OF DETERMINATION OF BREAKING BEHAVIOUR BY SETTING TIME (This Appendix forms an integral part of this Standard) K1_ SCOPE. This Appendix sets out a method for determining the setting time category of a mixture of aggregate and bitumen emulsion and subsequent classification of the emulsion. K2 MATERIALS. Three ypes of crushed aggregates are reqiitl as specified elow. Each aggregate shall be sieved to pass a 9.5 mm aperture size sieve complying with AS 1152 and be retained on a 4.75 mm aperture size sieve complying with AS 115: and shall be vashed and dried. 500 g baxches shall be prepared as follows: 400 g dolerite from Prospect quarry, N.S.W.* 0 g white quartz (indicator) from Tenterfield, N.S.W.* 50 g limestone (indicator) from Cow’s Flat, N.S.W.* K3 APPARATUS. The following apparatus is required: (@) Porcelain evaporating dish. A porcelain evaporating dish of approximately 230 mm diameter. (b) Non-metallic spatula. A non-metallic spatiia with a blade approximately 19 mm. ‘wide, rounded at both ends. (©) Balance, A balance of at least 2 kg capacity, accurate to 0.5 g. (@) Stopwatch or clock. Stopwatch or clock with seconds display. (©) Glass beaker. A glass beaker of 100 mL capacity, with lip and glass stirring rod. K4 TEST CONDITIONS. The test shall be carried out in a test room or compartment free from strong draughts and with atmospheric conditions maintained ata temperature of 232°C and relative humidity not less than 40 percent (see Note). Allow apparatus and materials to reach equilibrium with these conditions. NOTE: An air cabinet can be used in place ofan airconditioned test room. Openings shouldbe provided to allow acces for the operators arms to perform the mung process KS PROCEDURE. The procedure shall be as follows: (a) Place a $00 g charge of the test aggregates in the porcelain dish and spread flat. (b) Stir the sample of emulsion until thoroughly mixed, and weigh into the 100 mL beaker sufficient of the sample so that 35 2 g is delivered on pouring. (©) Pour 35 +2 g of emulsion as uniformly as possible over the test aggregate and, without delay, start the stopwatch and commence mixing in the following manner: (Turn the aggregates in from the edge to the centre at about two strokes of the spatula per second, i) For each stroke, push the spatula lengthwise into the aggregates in the dish to the full depth of the material and at an angle of about 30 degrees to the horizontal. iii) Cast the material towards the centre of the dish on each stroke by lifting and rotating the spatula, (iv) Between each stroke rotate the dish about 45 degrees in a constant direction. (4) Continue mixing for up to 3 min in the case of rapid setting emulsions, for 4 min to 7 min in the case of medium setting emulsions, and for a minimum of 8 min in the case of slow setting emulsions. (©) Inspect the mixture for any indications of breaking of the emulsion, such as— (balling up of thé aggregate by free bitumen; Gi) the presence of a ‘thin’ coating of bitumen, allowing the white indicator stone to show through; ii) a ‘watery’ appearance of the stone and a streakiness in the emulsion film ‘on the side of the dish; or ‘Stocks ofthese aggregates are avallable from the Engineer Manager, Central Asphalt Depot, Department of Main Roads, Granvile, NS.W ‘COPYRIGHT AS 11601988AS 1160—1988 K6 REPORT. Record the time in emulsion as follows— (a) rapid-setting type—if any one of the indications of breaking is apparent if mixing (b) medium-secting (ppe— (©) slow-setting type—if all pieces of aggregate are smooth 2 (Gv) presence of stone pick up when pressed with the spatula, indicating the presence of bitumen on both stone and spatula, NOTES: 1, Severe frothing sometimes develops during mixing, tending to mask the breaking of the emulsion ‘The presence Of Pick up asin Item en) san indication of emulsion break. 2. Usually, the onset of breaking ofthe emulsion is quite evident during mixing as isthe absence ‘of breaking a the end of mixing. Rapid setting grade of emulsion sually break after about? min. 5. The testi not designed to sea lower limit forthe rate of break but abnormally rapié breaking, 2 within 0.3 min, may indicate an unstable emulsion, further evidence of whieh should be Tooke fot inthe form of partial breaking during the sieve tes or viscosity determination. A sedimentation {est should aso be conducted in such sicumstance, 4 Push the spatula against the stones for about 2 seconds then withdraw and inspect stones which femain stuck to it and wil ot falloff. If here is only one layer of stone the end poi has not been reached but fone sone stick to another onthe spaule sat fete end pot. utes to the nearest 0.25 min, Classify the has proceeded for 3 minutes or less; any one of the indications of breaking is apparent if mixing has proceeded for at least 4 min or more but not more than 7 min; or and uniformly coated ing for 8 minutes. with emulsion, and no free bitumen is evident after mi ‘COPYRIGHT2 APPENDIX L PROCEDURE FOR RECOVERY OF RESIDUE FROM BITUMEN EMULSION (This Appendix forms an integrai part of this Standard) Lt SCOPE. This Appendix sets out a procedure for the recovery of residue from bitumen emulsion, for testing. 12 REAGENT. A 2:1 mixture of industial methylated spirit and water. 13 APPARATUS. The following apparatus is required: (a) Metal containers. Metal containers of alcut 0.5 L capacity, with a diameter of about 90 mm and depth about 105 mm, ita Jouble crimped base and side seams. Glass rods. Glass rods of approximately * mm diameter and about 180 mm. Tength, with flame polished ends. (©) Thermometer. A thermometer reading to 200°C, graduated in intervals of 1°C. (@) Balance. A balance having a minimum capacity of 250 g, accurate to 0.3 g and readable to 0.1 g, (©) Electric hotplate, An electric hotplate with an input control. (O Tongs or thermally insulated gloves. ‘Tongs or thermally insulated gloves to hold the metal containers. * (g) Shallow dish. A shallow dish to hold cooling water. (h) Carbon dioxide gas bottle. A carbon dioxide gas bottle with pressure regulator, connected by flexible wing through a 500 mL gas washing bottle, to a nozzle Of glass tubing having an internal diameter of about 6 mm. The nozzle shall ha the delivery end bent through approximately 180 degrees so that 1. may be hooked over the side of the metal container and extend down the inside about 50 mm. NOTE: The purpose ofthis apparatus io dtect the flow of gas down the inside ofthe container to form a non-ovidizing atmosphere without hindering the cape of volatile matter, () Sieve. A sieve with an aperture of 300 wm, complying with AS 1152. ®) 4 PROCEDURE. The procedure shall be as follows (2) Weigh to the nearest 0.1 g about 60 g of the thoroughly mixed sample in a tared metal container, in which a tared glass rod and thermometer clipped together hhave been placed. (©) Add 25 mL of the reagent and place the assembly on the hotplate. (©) Connect the gas nozzle, adjust the rate of flow of gas at about 2 bubbles per second (wien passed through gas washing bottle), and commence the evaporation process (@) Adjust temperature of the hotplate and in order to control boiling, rock the container from side to side with tongs while stirring. NOTE: It may be advantageous fo pace piece of wie gauze oer the hotplate as an aditonal, means of regulating the ate of heating but heir space caused by tered in of the bases usualy Mequate (¢) Remove container from the hotplate when frothing subsides and temperature rises 0 about 130°C. Cool to about $0°C by immersing the container in a shallow dish of water, maintaining the gas flow into the container. (D Remove gas nozzle, dry container, and weigh to the nearest 0.1 g. (g) Repeat evaporation with further additions of reagent until the loss in mass between successive evaporations is less than 0.2 8. ‘Add 25 mL of reagent, attach the gas nozzle and repeat evaporation procedure in Steps (a) to (F) above. NOTE: Repeted evaporation are usually required only in he cas of samples containing non aqueous volates () The residue obtained may be utilized to determine viscosity and insoluble matter siven in Table 1 ) coPyRIGHT AS 11601988PUBLICATIONS OF THE ASSOCIATION A list of Australian Standards may be purchased or inspected at ‘any office of the Association OFFICES OF THE ASSOCIATION Those interested in the work of the Association are invited to call at the Head Office or any Branch Office, or write for literature. : NEW SOUTH WALES: Head Office: Standards House, 80 Arthur Street, North Sydney, 2060. Mail: PO Box 458, North Sydney, 2059. Telex 26514. Facsimile (02) 959 3896 Neweastle Branch Office: 51 King Street, Newcastle, 2300. 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