1、July 2016 English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 75.160.20!%XLQ“2534146www.din.deDIN
2、ISO 10478Petroleum products Determination of aluminium and silicon in fuel oils Inductively coupled plasma emission and atomic absorption spectroscopy methods (ISO 10478:1994),English translation of DIN ISO 10478:2016-07Minerallerzeugnisse Bestimmung von Aluminium und Silizium in Kraft- und Brennsto
3、ffen Verfahren der optischen Emissionsspektrometrie mit induktiv gekoppeltem Plasma und der Atomabsorptionsspektrometrie (ISO 10478:1994),Englische bersetzung von DIN ISO 10478:2016-07Produits ptroliers Dtermination de laluminium et du silicium dans les combustibles Mthodes par spectroscopie dmissio
4、n plasma induit et spectroscopie dabsorption atomique (ISO 10478:1994),Traduction anglaise de DIN ISO 10478:2016-07www.beuth.deDocument comprises 10 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.07.16 A comma is used as the d
5、ecimal marker. Contents Page National foreword 3 Nationaler Annex NA (informative) Bibliography 3 1 Scope 4 2 Normative references 4 3 Principle 4 4 Reagents 5 5 Apparatus . 5 6 Probenvorbereitung . 6 7 Procedure . 6 7.1 Test portion . 6 7.2 Preparation of test solution . 6 7.3 Preparation of blank
6、solution . 7 7.4 Preparation of calibration solutions 7 7.5 Setting up and operationg the inductively coupled plasma atomic emission spectrometer . 7 7.6 Setting up and operating the atomic absorption spectrometer . 8 8 Calculation 9 9 Expression of results 9 10 Precision . 10 10.1 Precision data fo
7、r results determined by inductively coupled plasma emission spectroscopy 10 10.2 Precision data for results determined by atomic absorption spectroscopy 10 11 Test report . 10 DIN ISO 10478:2016-072 National foreword This document (ISO 10478:1994) has been prepared by Technical Committee ISO/TC 28 “
8、Petroleum products and related products of synthetic or biological origin” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-06-34 AA Anforderungen an H
9、eizle und Schifffahrtsbrennstoffe of the Fachausschuss Minerall- und Brennstoffnormung (FAM). Attention is drawn to the possibility that some elements of this document may be the subject of patent rights. DIN and/or DKE shall not be held responsible for identifying any or all such patent rights. For
10、 the purposes of this document, “% (m/m)” is used to express the mass fraction of a substance. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 648 DIN EN ISO 648 ISO 1042 DIN EN ISO 1042 ISO 3696 DIN ISO 3696 ISO 3819 DIN EN ISO 3819 IS
11、O 4788 DIN EN ISO 4788 National Annex NA (informative) Bibliography DIN EN ISO 648, Laboratory glassware Single-volume pipettes DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN EN ISO 3819, Laborator
12、y glassware Beakers DIN EN ISO 4788, Laboratory glassware Graduated measuring cylinders DIN ISO 10478:2016-073 Petroleum products - Determination of aluminium and silicon in fuel oils - Inductively coupled Plasma emission and atomic absorption spectroscopy methods WARNDNG - The use of this Internati
13、onal Standard may involve hazardous materials, operations and equipment. This Standard does not purport to address all of the safety Problems associated with its use. It is the responsibility of the User of this Standard to establish appropriate safety and health practices and determine the applicab
14、ility of regulatory limitations Prior to use. 1 Scope This International Standard specifies a method for determining the aluminium and Silicon contents of fuel oils at concentrations between 5 mg/kg and 150 mg/kg for aluminium and 10 mg/kg and 250 mg/kg for Silicon using inductively coupled Plasma e
15、mission and atomic absorption spectroscopy. ISO 1042:1983, Laboratory glassware - One-mark volume tric flasks. ISO 3696:1987, Water for analytical laboratory use - Specifica tion and test methods. ISO 3819:1985, Laboratory glassware - Beakers. ISO 478811980, Laboratory glassware - Graduated measurin
16、g cylinders. 3 Principle 2 Normative references The following Standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publi- cation, the editions indicated were valid. All Standards are subject to revision, and Parties
17、to agreements based on this International Standard are encouraged to investigate the possibility of applying the most re- cent editions of the Standards indicated below. Members of IEC and ISO maintain registers of cur- rently valid International Standards. ISO 648: 1977, Laboratory glassware - One-
18、mark pipettes. ISO 835-2:1981 B Laboratory glassware - Graduated pipettes - Part 2: Pipettes for which no waiting time is specified. A weighed quantity of homogenized Sample is heated in a clean platinum basin, the combustible material removed by burning and the carbon finally removed by heating in
19、a muffle furnace at a temperature of 550 “C + 25 “C. The residue is fused with a dilithium tetraboratellithium fluoride flux, the fused mixture di- gested in a Solution of tartaric acid and hydrochloric acid, and diluted to volume with water. The Solution is aspirated into either the Plasma of an in
20、ductively coupled Plasma emission spectrometer (ICPES), and the emission radiation of the resonance lines of aluminium/silicon measured and compared with that of Standard calibration solutions, or the flame of an atomic absorption spectrometer (AAS) and the absorption of the resonance radiation of t
21、he aluminium/silicon measured and compared with that of Standard calibration solutions. DIN ISO 10478:2016-074 0 ISO 4 Reagents During the analysis, use only reagents of recognized analytical grade and only water of at least grade 3 purity as specified in ISO 3696. 4.1 Potassium hydrogensulfate, (KH
22、SO,), fused solid. 4.2 Flux, mixture of 90 % (m/m) dilithium tetraborate 8 g of sodium hydroxide in a zirconium crucible fitted with a close-fitting lid (5.2) at dull red heat until a clear melt is obtained. Cool and dissolve the solidified melt in 100 ml of hydrochloric acid/water Solution (4.6.2)
23、in a 400 ml beaker (5.12). Cool, transfer and dilute the Solution quantitatively with water to 1 000 ml in a volumetric flask (5.8) followed by immediate transfer to a plastic bottle (5.14) for long-term storage. 5 Apparatus (Li,B,O,) and 10 % (m/m) lithium fluoride (LiF). 4.3 Propan-2-01. 4.4 Tolue
24、ne. 4.5 Toluene/propan-2-01 mixture (1 + 1). Mix one volume of toluene with one volume propan-2-01. 4.6 Hydrochlorit acid, concentrated, 36 % Laborstory apparatus and apparatus described in 5.1 to 5.15 shall be used. Clean all glassware carefully with hot hydrochloric acid (4.6.1) and rinse thorough
25、ly with water to eliminate contamination. 5.1 Platinum basin, 100 ml capacity, cleaned with molten potassium hydrogensulfate (4.1). of 4.6.1 Hydrochlorit acid Solution (1 + 1). NOTE 1 The following cleaning technique is rec- ommended: place 5 g of potassium hydrogensulfate (4.1) in the basin, heat i
26、n a muffle furnace at 550 “C f 25 “C or over a Bunsen burner for 5 min. Allow to cool, wash out with distilled or deionized water and dry. 5.2 Zirconium crucible, with a close-fitting zirconium lid, 30 ml to 50 ml capacity. Mix one volume of hydrochloric acid (4.6) with one volume of water. 4.6.2 Hy
27、drochlorit acid Solution (1 + 2). 5.3 Mixer, non-aerating, high-speed shear type. Mix one volume of hydrochloric acid (4.6) with two 5.4 Electric oven, capable of being maintained at a temperature between 50 “C and 60 “C. volumes of water. 4.7 Tartaric acid. 5.5 Electric muffle furnace, capable of b
28、eing main- tained at temperatures of 550 “C * 25 “C and 925 “C a dinitrogen Oxide (nitrous oxidejlacetylene burner; and a light detector with a Use either a ready-made commercially available sili- con Standard solution, 1 000 mg/l, or prepare by fus- ing 2,140 g of Silicon dioxide (99,99 % purity) w
29、ith DIN ISO 10478:2016-075 suitable measuring and readout System. The scale shall be linear in absorbance or in light intensity, or shall be directly in concentration units with curve cor- rection. preferably contain approximately 1,3 mg of alu- minium. NOTE 3 The mass of test Portion proposed, base
30、d on the aluminium content, will also suffice for the Silicon determi- 5.8 Volumetric flasks, 100 ml and 1 000 ml, com- plying with ISO 1042, class A. nation, as both elements are usually found in fuel oils as- sociated with each other. 5.9 Pipettes, 1 ml, 2 ml, 5 ml, 10 ml, 20 ml and 7.2 Preparatio
31、n of test solution 25 ml, complying with ISO 648, class A. 7.2.1 lmmediately after homogenization transfer the 5.10 Pipettes, 1 ml and 2 ml, graduated in 0,l ml subdivisions, complying with ISO 835-2. test Portion from the homogenized Sample to the weighed platinum basin (5.1); reweigh the basin and
32、 contents to the nearest 0,l g to obtain the mass of 5.11 Measuring cylinders, 10 ml, 25 ml, 50 ml and the test Portion taken. 100 ml, with subdivided graduations, complying with ISO 4788. 7.2.2 Warm the basin and contents gently with a Bunsen flame until the Sample ignites. Maintain the 5.12 Beaker
33、, 400 ml squat form, complying with ISO 3819. contents of the basin at a temperature such that most of the combustible material is removed and only car- bon and ash remain. 5.13 Filter Paper, “ashless”, 0,Ol % (m/m) ash NOTE 4 maximum. If the Sample contains considerable amounts of moisture, foaming
34、 and frothing may Cause loss of Sample. 5.14 Plastic bottles, unfilled virgin plastic, suitable for long-term storage of dilute acid solutions, 100 ml and 1 000 ml. 5.15 Balance, capable of being read to the nearest 0,2 mg. 6 Sample preparation If foaming and frothing occur, discard the Sample and t
35、o a fresh Portion add 1 ml to 2 ml of propan-2-01 (4.3) before heating. If foaming and frothing are not sufficently reduced, add 10 ml of a mixture of toluene/propan-2-01 (4.5) to a further test Portion and mix thoroughly. Place several Strips of ashless filter Paper (5.13) in the mixture and warm g
36、ently (when the Paper begins to burn, the greater patt of the water will have been removed). The Sample shall be homogenized thoroughly before the test Portion is taken. Place the Sample Container in an oven at a temperature between 50 “C and 60 “C and maintain the Sample at this temperature until a
37、ll the Sample has melted and reached a uniform viscosity. Insert the shaft of the mixer (5.3) into the Sample so that the head of the shaft is immersed to approximately 5 mm from the base of the Container. Homogenize the Sample for approximately 5 min. In the case of fluid samples which have stood u
38、ndis- turbed for several months, use a plastic rod to dis- lodge any Sediment adhering to the base of the Sample Container before homogenization. NOTE 2 Failure to wili invalidate results. 7 Procedure use this homogenization procedure 7.1 Test Portion The mass of test Portion taken from the Sample (
39、clause 6) shall weigh between 20 g and 50 g, and 7.2.3 Place the basin and contents in the muffle furnace (5.5) preheated to a temperature of 550 “C and that the sol- ution does not contain free fluoride “ion” above the 5 mg/1 Ievel. 7.3 Preparation of blank Solution Prepare a Zero-concentration Sol
40、ution containing only 0,4 g flux and 50 ml of the tartaric acid/hydrochloric acid Solution (4.7.1) diluted to 100 ml and transfer to a plastic bottle, 100 ml (5.14). 7.4 Preparation of calibration solutions The calibration solutions then contain 5 mg/l, 10 mg/l, 25 mg/1 and 50 mg/1 of Silicon respec
41、tively. 7.4.3 Storage Transfer all Standards to 100 ml plastic bottles (5.14). NOTE 9 When both aluminium and Silicon are being de- termined together, the 5 mg/1 to 50 mg/1 calibration sol- utions of each may be combined, providing there are no incompatibility Problems caused by the reagents used in
42、 the preparation of the Standard solutions 4.8.1 and 4.8.2. 7.5 Setting up and operating the inductively coupled Plasma atomic emission spectrometer 7.5.1 General Consult and follow the manufacturers instructions for the Operation of the instrument. NOTE 10 Design differentes between instruments, IC
43、P excitation sources and different selected analytical wave- lengths for individual spectrometers make it impracticable to specify the required manipulations in detail. 7.5.2 Peristaltic pump If using a peristaltic pump, inspect the pump tubing and replace it, if necessary, before starting each day.
44、 Verify the Solution uptake rate and adjust it to the desired rate. 7.4.1 Aluminium 7.5.3 ICP excitation Source Prepare a 250 mg/1 aluminium working solution by di- luting 25 ml of the 1 000 mg/1 Standard Solution (4.8.1) to 100 ml with water. To each of four clean 100 ml volumetric flasks (5.8) add
45、 0,4 g of the flux and 50 ml of the tartaric acid/hydrochloric acid sol- ution (4.7.1). To successive flasks add 2 ml, 4 ml, 10 ml and 20 ml of the 250 mg/1 aluminium working Solution and dilute to 100 ml with water. The calibration solutions then contain 5 mg/l, 10 mg/l, 25 mg/1 and 50 mg/1 of alum
46、inium respect- ively. Ignite the ICP excitation Source at least 30 min before performing an analysis. During this warmup period nebulize distilled or deionized water through the Plasma torch. NOTE 11 Some manufacturers may recommend even longer warmup periods. 7.5.4 Wavelength profiling Perform any
47、wavelength profiling that is called for in the normal Operation of the instrument. 7.4.2 Silicon 7.5.5 Operation Parameters Prepare a 250 mg/1 Silicon working Solution by diluting 25 ml of 1 000 mg/1 Standard Solution (4.8.2) to 100 ml with water. To each of four clean 100 ml volumetric flasks (5.8)
48、 add 0,4 g of the flux and 50 ml of the tartaric acid/hydrochloric acid Solution (4.7.1). To successive flasks add 2 ml, 4 ml, 10 ml and 20 ml of the 250 mg/1 Silicon working solution and di- lute to 100 ml with water. Assign the appropriate operating Parameters to the instrument task file so that it is possible to determine the desired elements. Include the following par- ameters: element, wavelength, background correction Points (optional), inter-element correcti
