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इंटरनेट मानक Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 15388 (2003): Specification for Silica Fume [CED 2: Cement and Concrete] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 15388:2003 Indian Standard SILICA FUME — SPECIFICATION ICS91.100. I5 0 BIS 2003 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 August 2003 Price Group 4 Cement and Concrete Sectional Committee, CED 2 FOREWORD This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Cement and Concrete Sectional Committee had been approved by the Civil Engineering Division Council. SiIica fume isvery fine pozzolanic material composed of ultra fine, amorphous glassy sphere (average diameter, 0.10-0. 15~m) of silicon dioxide (Si02) produced during the manufacture of silicon or ferro-silicon by electric arc furnaces at temperature of over 2 000”C. The micro silica is formed when SiO gas produced in the furnace mixes with oxygen, oxidizes to Si02, condensing into the pure spherical particles of micro silica that form the major part of the smoke or fume from the furnace. These fumes are collected and bagged called silica fume. It is also known as condensed silica fume and micro silica. The Committee also felt that chloride content in silica fume shall be declared by the manufacturer sothat different samples of silica fume can be compared and Engineer- in-Charge is in knowledge of the amount of chloride entering into concrete through silica fume. This standard has been formulated to fulfil the need for a specification for this material, in view of its increasing use in the country. [n the preparation of this standard, due weightage has been given to the international coordination among the standards and practices in different countries in addition to relating itto the practices in the field in this country. For this, assistance has been derived from the following: a) ASTM C 1240-2000 ‘Standard specification for use of silica fume as a mineral admixture in hydraulic cement concrete, mortar and grout’; issued by the American Society for Testing and Material b) EN 197-1:2001 ‘Cement — Part 1: Composition, specifications and conformity criteria for common cements’ The composition of the Committee responsible for formulation of the standard is given at Annex B. For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of atest, shall be rounded off in accordance with IS 2: 1960 ‘Rules for rounding off numerical values (revisecf)’. The number of significant places retained in the rounded off value shou]d be the same as that of the sp ecified value in this standard. IS 15388:2003 Indian Standard SILICA FUME — SPECIFICATION 1SCOPE Table 1Chemical Requirements (Clause 4) This standard covers the chemical and physical requirements of silica fume for use in concrete and other systems containing hydraulic cement. s] Characteristic Requirements Test Method 2 REFERENCES N (2) (3) (4) The following standards contain provisions which i) SiOz ,percentbymass, 85.0 IS 1727 Min through reference in this text, constitute provisions of ii) Moisture content, percent 3.0 see this standard. At the time of publication, the editions by mass, Max Note1 indicated were valid. All standards are subject to iii) Loss on ignition, percent 4.0 1S1727 revision and parties to agreements based on this bymass, J&x standard are encouraged to investigate the possibility iv) Alkalies asNalO, percent, 1.5 See of applying the most recent editions of the standards Max Notes indicated below. 2and 3 [S No. Title NOTES 1727:1967 Methods of test for pozzolanic 1For determination ofmoisture content, dry aweighed sample materials (@Wrevision) as received to constant mass in an oven at 105°C to 11O°C. Express inpercentage, the loss inmass and record as moisture 4082:1996 Recommendations on stacking and content. storage of construction materials and ZRequirement of limiting alkali shall be applicable incase components atsite (second revision) silica fume is to be used in concrete containing reactive 4305:1967 Glossary of terms relating to aggregate. pozzolana 3 For determination of alkalies, method of test used for 6491:1972 Methods of sampling fly ash determination ofthis incement maybe adopted. 3 TERMINOLOGY 5 PHYSICAL REQUIREMENTS 3.0 For the purpose of this standard, the definitions Silica fume shall conform to the physical requirements given in IS 4305 and the following shall apply. given in Table 2. 3.1 Silica Fume — Very fine pozzolanic material, 6SAMPLING AND CNTERIA FOR CONFERMfTY composed mostly of amorphous silica produced by electric arc furnaces as a byproduct of the production 6.1 Sampling of elemental silicon or ferro-silicon alloys. 6.1.1 The methods and procedure of sampling of silica fume shall be same as the method given for fly ash in 3.2 Silica Fume inNatural State — Silica fume taken IS 6491. All samples whether grab or composite shall directly from the collection filter. The bulk density have amass ofatleast 1kg. Two grab/~omposite samples typically being in the range of 150-350 kg/m3. shall be taken from the lot for the first 100 t of silica 3.3 Densitied Silica Fume — Silica fume that has been fume. For each subsequent 100 t from the lot of silica treated to increase the bulk density by particle fi.tme,one sample shall be taken. However, not less than agglomeration. The bulk density typically being above two samples shall be taken inany sampling programme. 500 kg/m3. 6.1.2 The sample or samples for the purpose of testing 3.4 Silica Fume Slurry — A homogeneous, liquid may be taken by the purchaser or his representative or suspension of silica fume particles in water, typically by any person appointed to supervise the work for the with a dry content of 50 percent by mass, purpose of which the silica fume is required or by the corresponding to about 700 kg/m3 of silica fume. latter’s representative. 4 CHEMICAL REQUIREMENTS 6.2 Criteria for Conformity Silica fume shall conform tothe chemical requirements 6.2.1 The samples of silica fume drawn in accordance given in Table 1. with 6.1 and then prepared as per 7and shall be tested as per 4 and 5. 1 IS 15388:2003 Table 2 Physical Requirements 7.2 Asampling device of appropriate size shall be used (Clause 5) totake material from the thoroughly mixed sample for purpose of making the test specimen. At least six random sub-samples shall be taken to prepare the test SI Characteristic Requi~e- Method of specimen. No. ment Test, Ref to r -! 8 STORAGE AND INSPECTION Annex IS No. 8.1 The silica fume shall be stored in such amanner so (1) (2) (3) (4) (5) as to permit easy access for proper inspection and identification of each consignment. i) Specific surface m:/g, 15 A Mirf(see Note I) 8.2 Adequate facilities shall beprovided tothepurchaser 11) Oversize percent 10 — 1727 for careful sampling and inspection, either atthe source retained on 45 micron IS or at the site of work, as may be specified by the Sieve, Max (see Note I) purchaser. For guidance on storage of silica fume atsite, iii) Oversize percent 5— 1727 IS4082 maybe referred to. Ingeneral, the material shall retained on45 micron IS be stored similar to cementifly ash storage depending Sieve, variation from upon the storage requirement in bags/bulk form. average percent, Max (see Notes Iand 2) 9 DELIVERY w) Compressive strength at 85.0 1727 7days aspercent of The supply of silica fume shall be m~de in suitable control sample, Mirr(see quantities mutually agreed upon between the purchaser Note 3) and the supplier. Where so required by the purchaser, NOTES the material shall be supplied in bags (jute laminated, I Any oqe ofthe tests specified in(i) or(ii) and (iii) indicated multiply paper or polyethylene lines). may headopted. 2For (iii) the average shall consist ofthe ten preceding tests or 10 MANUFACTURER’S CERTIFICATE all ofthe preceding tests ifthe number is less than ten. 3 Inthe test method fordetermination ofcompressive strength The supplier/manufacturer shall satisfy himself that the Ofsilica fume cement mortar in accordance with IS 1727, the silica fume conforms to the requirements of this \alue of factor N may be taken as one. standard and, if requested by the purchaser, shall furnish acertificate to this effect, indicating the results 6.2.1.1 Samples representing each 100tof silica fume of the tests carried out on the samples of silica fume. shall be tested for moisture content, loss on ignition and oversize. 11 MARKING 6.2.1.2 Testing for all other physical and chemical 11.1 Each bag/consignment of silica fume shall be requirements shall be carried out on composite samples clearly and permanently marked with the,<ollowing .. representing not more than 400 t material each. The information : composite samples shall be prepared by combining a) Identifications of the source of silica fume, portions equally from each of 100 t sample. b) Net mass of silica fume, 6.2.2 The lot shall be considered passing if samples c) Batch/Control unit number, meet in all the requirements. The silica fume may be d) Month and year of packing, and rejected if it fails to meet any of the requirements of e) Any other identification mark as required by this standard. In case of dissatisfaction with the results the purchaser. of tests, the producer or supplier may request re-testing of the failed consignment. 11.2 BIS Certification Marking 7 SAMPLE PREPARATION The silica fume may also be marked with the Standard Mark. 7.1 The grab orcomposite samples drawn inaccordance with 6.1 shall be mixed thoroughly. A clean and dry 11.2.1 The use of the Standard Mark is governed by laboratory concrete drum mixer provides adequate the provisions of the Bureau of Indian Standards Act, mixing for thepurpose. The amount of silica fume shall 1986 and the Rules and Regulations made thereunder. be 10to50 percent ofthe volume capacity ofthe mixer. The.details of conditions under which alicence for the The mixing time shall be 5 + 1 min. A polyethylene usei of the Standard Mark may be granted to film shall be secured on the drum to keep the material manufacturers or producers maybe obtained from the in the drum during mixing of the sample lot. Bureau of Indian Standards. 2 :,, IS 15388:2003 12 HEALTH AND SAFETY material. In many applications silica fume is handled asaaqueous slurry, redueing the dusiproblem virtually 12.1 Owing to its fineness and its high silicon dioxide to zero in such cases. content, fears have been expressed over the use of the powder forms of micro silica. A large number of 12.2 Similar information shall be provided in the X-ray diffraction analysis suggest that itisamorphous shipping invoices accompanying the shipment of bulk material and should therefore be less dangerous than a silica fume. crystalline material. However, it is advisable to take 12.3 The silica fume consignment shall be in good all necessary precautions while handling and using the condition at the time of inspection. ANNEX A (Table 2) DETERMINATION OF SPECIFIC SURFACE AREA BY GAS ADSORPTION USING THE BET METHOD A-1 SCOPE complete when a steady value of the residual gas This method of te’stspecifies the determination of the pressure p,of its composition or the sample mass mis total specific external and internal surface area of reached. disperse or porous solids by measuring the amount of A-3.2 Methods of Measurements physically adsorbed gas according to the method of Brunauer, Emmett and Teller (BET method). Adsorption isotherms may be obtained by volumetric, gravimetric, calorimetric or spectroscopic The BET method cannot reliably be applied to solids measurements or by the carrier gas method using which absorb the measuring gas. continuous or discontinuous operation. The procedure A-2 PRINCIPLE recommended by the manufacturer shall be followed. The method specified involves the determination of The adsorptive gas isadmitted to the sample container the amount of adsorbate or adsor ptive gas required to which is held at a constant temperature. The amounts cover the external and the accessi ble internal pore adsorbed are measured in equilibrium with the surfaces of a solid with a complete monolayer of adsorptive gas pressure p and plotted against relative adsorbate. This monolayer capacity can be calculated pressure, Plpo,to give an adsorption isotherm. from the adsorption isotherm using the BET equation. A-4 EVALUATION OF ADSORPTION DATA Nitrogen at its boiling point (about 77 K) is usually the most suitable adsorptive. The amount of gas adsorbed n~,preferably expressed in moles per gram, is plotted as ordinate against the A-3 PROCEDURE respective pressure, plpoas abscissa to give the A-3.1 Sample Preparation adsorption isotherm. The monolayer capacity n~ is calculated using the BET equation. Prior to the determination of an adsorption isotherm, remove physically adsorbed material from the sample PIPO _ 1 +C—–l. —p surface by degassing, while avoiding irreversible changes to the surface. As certain the maximum ‘, [l–(P/PO)] ‘mC ‘mc P() temperature at which the sample is not affected by where rhermogravimetric analysis or by trial experiments using different degassing conditions of time and P= pressure of the adsorptive in equilibrium temperature. When vaccumed conditions are used, with the adsorbate, Pa; degassing to aresidual pressure of approximately 1Pa Po = saturation vapour pressure of the or better is usually sufficient. Degassing of a sample adsorptive, Pa; can also be performed at elevated temperature by n= specific amount adsorbed, mol g-’; flushing with helium or with adsorptive. Degassing is a 3 IS 15388:2003 ?1 = specific monolayer capacity ofadsorbate; static or continuous gas admission, single- m amount of adsorbate needed to cover the point determination, calibration of dead surface with a complete monolayer of volume or buoyancy; molecules; and f-) Adsorptive (chemical nature, purity, moisture C = BET parameter. content); A-5 TEST REPORT g) Adsorption isotherm (n~,expressed, inmol g-l, plotted against relative pressure, p/pO),sample The report of the determination shall include the temperature in kelvin, saturation vapour following information : pressure, expressed in Pa); a) Laboratory, type of equipment, date of h) Evaluation parameters: multipoint or single- determination; point determination, BET plot or range of b) Characterization of the sample, for example linearity, monolayer capacity n,”expressed in source, chemical composition, purity, method mol g-], C value, molecular cross-sectional of sampling, sample division; area amexpressed in square nanometers; c) Pre-treatment and degassing conditions, for j) Specific surface area, a,, expressed in m’lg; example temperature, residual pressure, and partial pressures, duration of degassing, k) Reference material(s) used for validation of flushing with adsorptive or helium, mass results. reduction; A-6 USE OF REFERENCE MATERIAL d) Mass of degassed sample, in g; e) Experimental procedure for adsorption To ensure proper working conditions and correct data isotherm determination, for example evaluation, the apparatus performance should be volumetric, gravimetric, chromatographic, monitored periodically using a certified surface area reference material. I ANNEX B (1’oreword) COMMITTEE COMPOSITION Cement and Concrete Sectional Committee, CED 2 Organization Representative(s) In personal capacity (‘Chandrika’ at 15’hCross, 63-64, East Park Road, DR H. C. VMVESVARAY(AChairman) Mallesu,aram, Bangalore-560003) B.G. Shirke Construction Technology Limited, Pune SHRIG. R. B}{ARITKAR Builders Association of India, Mumbai SECRETARY Building Materials & Technology Promotion Council, New Delhi SHRIT. N. G(JPTA SHJUJ. K. PRASAD(Alternate) Cement Corporation of India Limited, New Delhi SHRIMAHESHKUMAR SHKI1.K. WAITAL(A/terns/e) Central Board of Irrigation and Power, New Delhi MEMBERSECRBTARY DIRECTOR(CIVIL)(Ahernate) Central Building Research Institute, Roorkee DRC. L. VERMA DRB. K. RAO(Alternate) Central Public Works Department, New Delhi CHIEFENGINEER(DESIGN) SUPERINTENDINEGNGINEER(S&S) (Alternate) Central Road Research Institute. New Delhi HEAO DIRECTOR(Alternate) Central Soil and Materials Research Station. New Delhi DIRECTOR SHIUP. L. KASHYAP(Alternate) Central Water Commission, New Delhi DIRECTOR(CMDD) (N&W) DEPUTYDISECTOR(CMDD) (NW&S) (Ahernate) Directorate General of Supplies & Disposals, Bangalore SHRIV. BALSUBIWMANIAN SHRJR. P. SINGH(Alternafe) Engineer-in-Chief’s Branch, Army Headquarters, New Delhi MAJGENYASNMALHOTRA SHIUMAHFNDRAPRASAD(Alternate) Fly Ash Mission, Department of Science & Technology, New Delhi DRVIMALKUMAR SHRIMUKf3HMATHUR(Alternate) Gammon India Limited, Mumbai SHRIS. A. RE~OI SHRIM. U. SHAH(Alfernafe) Geological Survey of India, Jaipur DR S. S. AMETA DRD. K. RAI(Alternate) Grasim Industries Limited, Mumbai SHRIA. K. JAJ~ COLSUDHIRTAMHANEY(RETD)(A/terns/c) Gujarat Ambuja Cements Limited, Ahmedabad SHRJJ. P. DESAI SHRIB. K. JAGETIA(Alternate) Hospital Services Consultancy Corporation (India) Ltd, Noida SHRIJ. SARUP SHRIP. K. JAIPURIAR(Alternate) Housing and Urban Development Corporation Limited, New Delhi SHRIV. SURESH SHRIV. ARULKUMAR(Alternate) Indian Concrete institute, Mumbai SHRIL. N. APTE SHRID. SRINIVASAN(Alternate) Indian Institute of Science, Bangalore PROFT. S. NA~ARAJ [ndian Institute of Technology, Roorkce PROFA. K. JAIN Indian Institute of Technology, Kharagpur DR ASHOKKUMARGHOSH Indian Roads Congress, New Delhi DR S. S. SEHJLA SHRIARUNKUMARSHARMA(Alternate) Institute for Solid Waste Research & Ecological Balance, DR N. BHANUMATHIDAS Vishakhapatnam SHIUN. KALIDAS(A/ternate) (Continued onpage 6) 5