DOCUMENT DESPATCH ADVICE. Biodiesel, Diesel Fuel Blend ( B6 to B20) Specification

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1 DRAFT IN WIDE CIRCULATION DOCUMENT DESPATCH ADVICE REF: DATE Technical Committee: Petroleum and Related Products Sectional Committee, PCD 3 Dear Sir, i) All interested members of PCDC ii) All members of Petroleum Lubricants and Related Products Sectional Committee, PCD 3; iii) All others interested. Please find enclosed the following documents: Doc:PCD 3(2865)C Doc: No. PCD 3( 2865)C Title Biodiesel, Diesel Fuel Blend ( B6 to B20) Specification Kindly examine this draft and forward your views stating any difficulty which you are likely to experience in your business or profession, if this is finally adopted as a revised standard. Last date for comments is : 02 October 2015 Comments if any, may please be made in the format as given overleaf and mailed to the undersigned at the above address. The document is also hosted on BIS website Thanking you, Encl: As above. Signature : Name : N K Kansara Designation Sc.F & Head (PCD) pcd@bis.org.in; chitra@bis.org.in

2 FORMAT FOR SENDING COMMENTS ON BIS DOCUMENTS (Please use A4 size sheet of paper only and type within fields indicated. Comments on each clauses/subclauses/table/fig. etc be started on a fresh box. Information in Column 4 should include reasons for the comments and suggestions for modified wording of the clauses when the existing text is found not acceptable. Adherence to this format facilitates Secretariat s work) Doc. No.: TITLE: LAST DATE OF COMMENTS: 02 October 2015 NAME OF THE COMMENTATOR/ORGANIZATION: Sl. No. Clause/Subclause/ para/table/fig. No. commented Commentator/ Organization/ Abbreviation Type of Comments (General/Editorial/ Technical) Justification Proposed change

3 व य पक पर न मस द तकन क सम तत प स ड 3 र ष त स दभभ प स ड 3( 2865)स रल ख र षण स ञ पन ददन क प र ल यम तकन क सम तत, प स ड 3 क समस त सदस य प स ड 3 क सभ उपसलमततय प र ल यम,क य एव स ब ध त उत प द षवभ ग पर द ( प स ड स )क सदस य ध खन व सभ तनक य मह दय /मह दय, रम स य क य आपक अव कन ह त तन नल खखत मस द स न ह : मस द स य व षय 1. प स ड 3 (2865 )स )ब -6- ब -20(- ब य ड ज, ड ज न लमरण - षवल ट क पय इस मस द क अव कन क अपन स मततय यह बत त ह ए भ ज कक यदद अ तत यह म नक मस द र य म नक क प म रक ल त ह ज य त इस प अम क न म आपक यवस य अथव क ब म य कद न ईय आ सकत ह स मततय भ जन कक अ ततम ततथ : 02 O to er 2015 स मततय क पय स न र प म अ ह त ष क भ ज न यव द, भवद य एन क क स व ञ तनक एफ एव रम ख(प स ड ) रतत उपर ल खखत म : pcd@bis.org.in, chitra@bis.org.in

4 For comments Only Doc: PCD 3( 2865)C Draft Indian Standard Biodiesel, Diesel Fuel Blend ( B6 to B20) Specification Se em e 2015 ICS No Last date for comments 02 O ber 2015 FOREWORD (formal clauses will be added later) The high speed diesel fuel continues to be the main fuel in India for public and commercial transport and this trend is expected to continue with demands to maximize its production to cater to the ever increas ing requirements of consumers. At national level the major part of the demand is met through import of crude from diverse sources as the domestic crude oil is able to meet only about 20% of the demand. Renewable energy sources are indigenous, nonpolluting and virtually inexhaustible and India is endowed with abundant renewable energy sources. Therefore, their use is required to be encouraged in all possible ways. Biodiesel is one such renewable and alternative fuel which can be used as standalone or its blend in diesel fuel as clean fuel. Currently blending of biodiesel in the high speed diesel is permitted under IS 1460 :2005 Automotive Diesel fuel. However, its proportion has been limited to 5 percent which is considered as not having any adverse impact compared to HSD alone on the vehicle performance. In order to provide the use of higher quantities of blends (B6 to B20)there is a need to prepare standard for B6 to B20 blend diesel fuel specification as with highe concentration of biodiesel in diesel ould have significant impact on me properties of pure diesel fuel. Since biodiesel is very clean fuel with less than 10 ppm of sulfur it would significantly reduce the vehicular emissions. The properties of commercial B6 to B20 blends depend on the refining practices employed and the nature of the distillate fuel oils and biodiesel from which they are produced. Distillate fuel oils, for example, may be produced within the boiling range of 150 C and 400 C having many possible combinations of various properties, such as volatility, ignition quality, viscosity, and other characteristics. Biodiesel, for example, can be produced from a variety of animal fats or vegetable oils that produce similar volatility characteristics and combustion emissions with varying cold flow properties. This draft standard describes specification for blends of more than 6% (v/v) and upto to 20% (v/v) of FAME in diesel fuel to be used in captive fleet application for designated vehicles. This fuel is not suitable for all vehicles, consult vehicle manufacturer or manual before use. Accordingly, the requirements of B6 to B20 diesel fuel for suitably designed vehicles meeting Bharat Stage III and Bharat Stage IV Emission Norms are furnished in Table l. A test method for estimating bio-diesel(fame) content has been stipulated in Annex B. This method has been developed on six bio-diesel samples (karanjia, soyabean, Jatropa, ricebran and palm oil ). Since the absorptivity of all t he bio-diesel is found to be almost same ( ) the method is independent of the nature of the bio d iesel. Considerable assistance has been drawn from ASTM D , standard specification of B6 to B20 diesel fuel and draft European specification EN for B20 while preparing this standard.

5 Draft Indian Standard Biodiesel, Diesel Fuel Blend ( B6 to B20) Specification 1 SCOPE 1.1 This specification covers fuel blend grades of 6 to 20 percent (v/v) biodiesel meeting IS15607 specification with remainder being a middle distillate diesel fuel (see IS 1460), collectively designated as B6 to B20. These BSIII & BSIV blended grades are suitable for various type of suitably designed diesel engines. 1.3 This specification prescribes the requirements, sampling procedure and test methods for B6 to B20 biodiesel blends at the time and place of delivery. It is applicable to automotive diesel fuel for use in diesel engine vehicles designed to run on B6 to B20 diesel fuel. It also find application with non automotive engines also. 2 REFERENCES The standards as given in Annex A contain provisions, which, through reference in this text, constitute provisions of this standard. At the time of publication the editions ind icated were valid. All standards are subject to rev ision and parties to agreements based on the standard arc encouraged to investigate the possibility of applying the most recent editions of the standards. 3 REQUIREMENTS 3.1 General The blended fuel shall be hydrocarbon oils of light middle or middle distillate grade diesel conforming to IS 1460 blended with biodiesel(6 to 20 volume percent) The use of fuel additives is permitted in order to improve the performance quality. Suitable fuel additives without known harm fu l side-effects are recommended in appropriate concentration to help to avoid deterioration of drivability and emissions control durability. Antioxidant/Stabilizing agents, as required, shall be incorporated The biodiesel blend(b6 to B20) shall be visually free of undissolved water, sediment and suspended matter. It shall also be free of any adulterant or contaminant that may render the fuel unacceptable for its commonly used applications B l e n d e d fuel shall not contain any residuum oi l Bio-diesel from 6 to 20 percent (v/v) may be blended with automotive d iesel fuel [ see Table 1, SI No. (xvi)] The use of dyes or markers is permitted. 3.2 The fuel shall also comply with the requirements given in Table 1 when tested according to the methods prescribed in col 4 and 5 of Table 1. 4 PACKING AND MARKING 4.1 Packing The fuel shall be packed and supplied in suitable containers as agreed to between the 5

6 purchaser and the supplier and subject to the provision of Red Tariff No. 18 Rules and Rates for the Conveyance by Rail of Explosives and Other Dangerous Goods, issued by the Indian Railway Conference Association, with any alternations or additions made thereafter. 4.2 Marking Each container shall be marked with the following information : a) Name of the material; b) Indication of the source of manufacture, initials or trade-mark, if any; c) Volume of the contents, in litres; d) Declaration of blend content e) Lot/Batch No f) Month & Year of manufacture or packing; and g) The C aution label 'FLAMMABLE' together with the corresponding symbol for labeling dangerous goods as given in Fig. 5 of IS 1260 (Part l). 4.3 BIS Certification Marking The container may also be marked with the Standard Mark. 4.3.l The use of the Standard Mark is governed by the provisions of the Bureau of Indian Standards Act, 1986 and the Rules and Regulations made there under. The details of conditions under which the licence for the use of the Standard Mark may be granted to manufactures or producers may be obtained from the Bureau of Indian Standards. 5 SAMPLING Representative samples of the material shall be drawn as prescribed in IS 1447 (Part 1). Table l Requirement for B6 to B20 Biodiesel Blend Fuel (Clauses and 3.2) Sl. No Characteristics Requirements Method of Test, Ref to ISO/ASTM D/ IP/EN [P:] of 1448/ /Annex (1) (2) (3) (4) (5) i) Density 1) at 15 0 C ISO 12185/3675 (kg/m 3 ) / D [P:16]/[P : 32 ] ii) Kinematic 40 0 C (cst) ISO3104 [P:25] iii) Flash point, Abel ( 0 C) Min 35 [P : 20] 6

7 iv) Sulphur 2) (mg/kg), Max BS III BS IV v) Carbon Residue (Ramsbottom) 3 on 10% residue,% mass) Max vi) Ash content (% mass) Max 0.01 vii) Water, ppm, Max 260 viii) Cu corrosion, 50 0 C, Max 1 ix) Cetane No 4), Min 51 x) Cetane index 4), Min 46 xi) PAH, m/m Max 11 xii) Lubricity, wear scar Diameter(wsd1.4) at deg C, micron, Max xiii) Acid No, mg of KOH/gm Max 0.2 D 4294/D 5453/ISO 20846/ ISO 20884/ISO D 4530/ ISO [P : 8] ISO 6245 [ P : 4/Sec 1] ISO 6296 /ISO [ P : 40 ] ISO 2160 [P : 15 ] ISO 5165 [ P : 9 ] ISO 4264/D4737 EN 12916/ IP391 ISO ISO 7537 [P: 1/Sec1] xiv) Oxidation stability, at 110 C, h, Min 20 EN15751 xv) Distillation, percent recovery at C Min. 95 xvi) Biodiesel Content, percent,v/v 6-20 ISO 3405 P:18 EN Annex B xvii) Pour point 5), Max Winter Summar 3 0 C 15 0 C D5949 / D5950/ D5985/ISO 3016 [P : 10/Sec 2] xviii) Cold filter plugging point(cfpp 5) Max Winter Summar 6 0 C EN 16329/D6371 [P:110] 7

8 18 0 C xix) Total contaminant, mg/kg Max 24 EN ) In case of dispute [ P:32 ) shall be the referee test method 2 ) In case of dispute, ASTM D 4294 shall be the referee test method. 3) This limit is applicable prior to addition of ignition improvers, if used. In case a value exceeding the limit is obtained on finished fuels in the market, ASTM D 4046/ ISO shall be used to establish the presence of nitrate containing compound. In such case the present limit for carbon residue cannot be applied. However, the use or ignition improver docs not 'exempt the manufacturer from meeting this requirement prior to the addition or additives. 4) For fuel processed from Assam crude, cetane number and cetane index is relaxed by 3 units. 5 ) Winter shall be the period from November to February in central and northern plains of India (both months inclusive) and rest of the months of the year shall be called as summer ANNEX A (Clause 2) Standard No List of Standards referred in the Standards Title 1260 ( Part I ) : 1973 Pictorial marking for handling and labeling of goods: Part I Dangerous goods (first revision) 1460 : 2005 Automotive diesel fuel Specification (fifth revision) 1447 (Part 1) : 2000 Petroleum and its products Methods of sampling Part 1 manual sampling(first revision) 1448 Methods of test for petroleum and its products [ P : 1/ Sec 1] :2002 Determination of acid number of petroleum products by potentiometric titration (second revision) [P : 2] : 2007/ ISO 6619:1988 Petroleum products and lubricants - Neutralization number - Potentiometric titration method (second revision) [P : 4/Sec 1] : Ash, sulphated ash and water soluble ash (third revision) 2008/ISO 6245 : 2001 [P: 8]:2012/ ISO 4262 Part 8: Carbon residue by Ramsbottom method (first revision) : 1993 [P 9] : 2013/ISO 5165 Cetane number (first revision) [P: 10/Sec 2] : 2013 / Cloud point and pour point: Section 2 Determination of pour point ISO 3016:1994 (second revision) [P:12]:2013 / ISO 2049:1996 [P : 15] : 2004/ISO 2160:1998 Colour by ASTM colour scale (first revision) Corrosiveness to copper - Copper strip test (third revision) 8

9 [P : 16] :1990 Density, relative density or API gravity to crude petroleum and liquid petroleum products by hydrometer method (third revision) [P: 18]:1991 Distillation of petroleum products (second revision) [P : 20] : 1998 Determination of flash point by Abel apparatus (second revision) [P : 25] :1976 Determination of kinematic and dynamic viscosity (first revision) [P : 32] : 1992 Density and relative density (second revision) [P : 40] : 1987 Water by distillation (third revision) [P :110] : 1981 Determination of cold filter plugging point of distillate fuels ISO 3405 ISO 3016 Petroleum products -- Determination of distillation characteristics at atmospheric pressure Petroleum products -- Determination of pour point ISO 6296 Petroleum products -- Determination of water -- Potentiometric Karl Fischer titration method ISO Petroleum products -- Determination of water -- Coulometric Karl Fischer titration method ISO 4264/ Petroleum products -- Calculation of cetane index of middle-distillate fuels by the four-variable equation ISO 3675 Crude petroleum and liquid petroleum products Laboratory determination of density Hydrometer method ISO Diesel fuel -- Assessment of lubricity using the high-frequency reciprocating rig (HFRR) -- Part 1: Test method ISO Crude Petroleum and Petroleum products - Determination of density - Oscillating U-tube method ISO 3104 Petroleum products -- Transparent and opaque liquids -- Determination of kinematic viscosity and calculation of dynamic viscosity ISO Petroleum products -- Determination of carbon residue -- Micro method ISO Methods of test for petroleum and its products: determination of low concentration of sulphur in automotive fuels energy-dispersive x- ray fluorescence spectrometric method ISO 7537 Petroleum products Determination of acid number Semi-micro colour-indicator titration method ISO Petroleum products -- Determination of sulfur content of automotive fuels -- Ultraviolet fluorescence method ISO Petroleum products -- Determination of sulfur content of automotive fuels -- Wavelength-dispersive X-ray fluorescence spectrometry ASTM D 4294 Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry 9

10 ASTM D 4530 ASTM D4737 ASTM D 5453 ASTM D5949 ASTM D5950 ASTM D5985 ASTM D 6371 Standard Test Method for Determination of Carbon Residue (Micro Method) Standard Test Method for Calculated Cetane Index by Four Variable Equation Standard Test Method for Determination of Total Sulfur in Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel Engine Fuel, and Engine Oil by Ultraviolet Fluorescence Standard Test Method for Pour Point of Petroleum Products (Automatic Pressure Pulsing Method) Standard Test Method for Pour Point of Petroleum Products (Automatic Tilt Method) Standard Test Method for Pour Point of Petroleum Products (Rotational Method) Standard Test Method for Cold Filter Plugging Point of Diesel and Heating Fuels EN12662 EN 12916/ EN EN15751 EN16329 IP391 Liquid petroleum products. Determination of total contamination in middle distillates, diesel fuels and fatty acid methyl esters Petroleum products. Determination of aromatic hydrocarbon types in middle distillates. High performance liquid chromatography method with refractive index detection Liquid petroleum products. Determination of fatty acid methyl ester (FAME) content in middle distillates. Infrared spectrometry method Automotive fuels. Fatty acid methyl ester (FAME) fuel and blends with diesel fuel. Determination of oxidation stability by accelerated oxidation method Diesel and domestic heating fuels. Determination of cold filter plugging point. Linear cooling bath method Petroleum products - Determination of aromatic hydrocarbon types in middle distillates - High performance liquid chromatography method with refractive index detection ANNEX B [Table l, SI No. (xvi)] ESTIMATION OF BIO-DIESEL CONTENT IN BLENDS OF DIESEL AND BIO- DIESEL BY FTlR SPECTROSCOPY TECHNIQUE B-1 SCOPE The method describes the methodology for the estimation of bio-diesel(fame) in diesel by using infrared spectroscopy.it is applicable to concentration from 1 to 20% volume. 10

11 B-2 SU MMARY OF THE METHOD The IR spectra of the sample is recorded in a fixed path length cell (0.05 mm) and absorbance area is measured in the region I cm 1 which is then compared with calibration curve developed using blends of known concentrations. The amount of biodicsel in diesel is then calculated using the calibration equation. B-3 SIGNIFICANCE AND USE The method can be used for quick quality checks on bio-diesel content estimation. It has specific use in the blends of diesel and bio-diesel being used commercially. B-4 APPARATUS B-4.1 Instrument - Infrared spectrophotometer covering the full range of cm 1 with linear absorbance versus linear wave number recording is required. Ordinate repeatability and accu racy of the inst ru ment shou ld be better than I percent of the full scale. The instrument should be i n a position to calculate the area under the peaks. B-4..2 Cells - Fixed path length cells with KBr windows and PTFE stoppers, having a path length of approximately 0.05-mm. B-4.3 Syringe - 1 ml syringe with luer fitting. B-5 CHEMICALS AND REAGENTS B-5.1 Cyclohexane -Spectroscopic grade. B-5..2 Chloroform -Spectroscopic grade. B-5.3 Bio-diesel Samples B-5.4 Commercial Diesel (see IS 1460) B-5.5 Benzene -Spectroscopic grade. B-6 PROCEDURE The calibration equation using known blends of bio-diesel samples as reference as given below can be developed and use the generated calibration equation for the estimation of bio-diesel content in unknown samples. Alternately, one can use the calibration equation provided for the estimation of bio-diesel content directly from the IR spectra of the unknown bio-diesel samples. B-6.l Reference Standards Prepare standard blends of bio-diesel in a commercial diesel sample in the range of 1-20 percent by volume. Accurately pipette the bio-diesel into 10-m1 volumetric flask.. Make up the volume with diesel to calculate the volume percent of the blends. B-6.2 Determination of Cell Path Length B Fill the IR cell with spectroscopic grade benzene and record the infrared spectrum over the whole range ( cm 1 ). B Measure the absorbance at 1960 cm 1 for cells having path length less than 0.1 mm. 1 1

12 B Cell thickness in mm = 0.1 x absorbance. B Calculate the cell path length correction factor to make the path length 0.05 mm. B-6.3 Calibration Equation B- 6.3.l Fill the cell using the syringe and taking care that there are no entrapped air bubbles. See that the exterior of the cell does not become contaminated. Fix the PTFE stoppers to the inlet and outlet of the cell. B Measure the area under the curve in the region cm 1 and plot these values (in the X-axis) against the known concentrations of bio-diesel in diesel (in the Y- axis) to obtain the calibration curve and the equation. Record the IR spectra of the known blends in MID-IR region. B-6.4 Record the IR spectra of the diesel sample with unknown concentration of biodiesel in diesel in the similar manner. Measure the area under the curve in the region cm 1 B-6.5 From the calibration curve, determine the concentration of the bio-diesel in unknown sample by using the calibration (regression) equation. B-7 Alternately, the combined calibration equation obtained for different bio-diesel samples (from Palm Oil, Jatropa Oil and Sunflower Oil) is given below: Y = l X where Y = concentration of unknown bio-diesel in volume percent, and X = area under the curve between the region I cm -1 in 0.05 mm cell path length of unknown sample B-7.1 Record the IR spectrum of unknown bio-diesel samples using pre-calibrated fixed path IR cell in cm -1 region and measure the area of the band in the region as described earlier. B-7.2 Determine the concentration of the bio-diesel in unknown sample employing the above equation. B-8 PRECISION The precision of the method is estimated employing the standard statistical techniques. Samples are prepared in the concentration range of 1-20 percent bio-diesel in diesel. The samples are analyzed by two operators in duplicate. ANOVA analysis is carried out on the results obtained and the precision statement of repeatability and reproducibility values are found to be 0.8 and 1.8 respectively. B-9 REPEATABILITY 5.1 to 20.0 percent volume

DOCUMENT DESPATCH ADVICE. Technical Committee: Petroleum and Related Products Sectional Committee, PCD 3

DOCUMENT DESPATCH ADVICE. Technical Committee: Petroleum and Related Products Sectional Committee, PCD 3 DRAFT IN WIDE CIRCULATION DOCUMENT DESPATCH ADVICE REF: DATE Doc:PCD 3(2867)C 02 09 2015 Technical Committee: Petroleum and Related Products Sectional Committee, PCD 3 i) All interested members of PCDC