DIN 51444-2003 Testing of petroleum products - Determination of nitrogen - Oxidative combustion method with chemiluminescence detector《石油产品的试验 氮含量测定 使用化学发光检测器的氧化燃烧法》.pdf
《DIN 51444-2003 Testing of petroleum products - Determination of nitrogen - Oxidative combustion method with chemiluminescence detector《石油产品的试验 氮含量测定 使用化学发光检测器的氧化燃烧法》.pdf》由会员分享,可在线阅读,更多相关《DIN 51444-2003 Testing of petroleum products - Determination of nitrogen - Oxidative combustion method with chemiluminescence detector《石油产品的试验 氮含量测定 使用化学发光检测器的氧化燃烧法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、 No part of this translation may be reproduced without the 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).Ref. No. DIN 51444 : 2003-11English price group 6 Sales No. 010602
2、.05Continued on pages 2 to 4.ICS 75.080Prfung von Minerallerzeugnissen Bestimmung des gebundenen Stickstoffs Verbrennungsverfahren mit Chemolumineszenz-DetektorIn keeping with current practice in standards published by the International Organization for Standardization (ISO), a comma has been used t
3、hroughout as the decimal marker.51444Determination of bound nitrogen in petroleum products by combustion and chemiluminescenceTranslation by DIN-Sprachendienst.In case of doubt, the German-language original should be consulted as the authoritative text.DEUTSCHE NORM November 2003ForewordThis standar
4、d has been prepared by Technical Committee Prfung von ssigen Kraftstoffen und Heizlen of the Fachausschuss Minerall- und Brennstoffnormung of the Normenausschuss Materialprfung (Mate-rials Testing Standards Committee).1 ScopeThe method specied in this standard serves to determine bound nitrogen in c
5、oncentrations ranging from about 0,3 mg/kg to about 300 mg/kg in petroleum products having a boiling range of 50 C to 400 C and viscosities between 0,2 mm2/s and 10 mm2/s at ambient temperature. Samples having a higher nitrogen content shall be diluted as appropriate prior to the analysis.2 Normativ
6、e referencesThis standard incorporates, by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and the titles of the publications are listed below. For dated references, subsequent amendments to or revisions of a
7、ny of these publications apply to this standard only when incorporated in it by amendment or revision. For undated references, the latest edition of the publication referred to applies.DIN EN ISO 4259 Petroleum products Determination and application of precision data in relation to methods of test (
8、ISO 4259 : 1992 + Corr 1 : 1993)3 PrincipleA sample is injected into a stream of carrier gas composed of an inert gas or a mixture of an inert gas and oxygen, evaporated and conveyed into a high-temperature zone where the bound nitrogen reacts with oxy-gen to form nitrogen monoxide (NO). Reaction wi
9、th ozone converts the latter into excited nitrogen dioxide (NO2), which emits light that can be detected by a photomultiplier. The resultant signal is a measure of the nitrogen content of the sample.4 DesignationDesignation of the method of determining bound nitrogen by chemiluminescence:Test DIN 51
10、444Page 2DIN 51444 : 2003-115 Apparatus5.1 Test assemblyThe test assembly shall be as shown schematically in gure 1. It is to be made up of the following.5.1.1 Furnace, capable of maintaining a temperature sufcient to evaporate the entire sample material and oxidize the bound nitrogen to form nitrog
11、en monoxide. The furnace temperature is to be specied by the manufacturer.5.1.2 Quartz combustion tube, for evaporating or pyrolysing the sample in a carrier gas and burning it with oxygen in a zone large enough to completely oxidize the sample. The tube inlet shall be sealed (e.g. with a septum). O
12、ther combustion tubes may be used if this does not adversely affect the precision of the method.Figure 1: Test assembly (schematic)5.1.3 Dryer, for drying the reaction products prior to the analysis using a chemical desiccant, permeation drying or a combination of both, since water vapour damages th
13、e detector.5.1.4 Chemiluminescence detector, capable of measuring the light emitted by the reaction of nitrogen monoxide and ozone.5.1.5 Evaluation unit with integrator.5.1.6 Microlitre syringes, having a nominal capacity of 5 l to 250 l and a needle long enough for its tip to extend into the hottes
14、t part of the evaporator zone during injection.5.1.7 Automatic sample injection system (optional), having reproducible injection speeds and consequently resulting in optimum combustion.5.1.8 Combustion boat for sample application (optional), for use with samples that may react with the needle, the p
15、yrolysis tube being designed in this case to allow the boat to be introduced into the combustion zone completely.5.1.9 Outlet unit of combustion tube (optional), capable of accommodating a removable quartz insert tube.5.1.10 Quartz insert tube (optional), lled with copper oxide, CuO, to promote comp
16、lete oxidation of sample.6 ReagentsUnless otherwise specied, analytical grade reagents shall be used.6.1 Chemically inert desiccant (e.g. magnesium perchlorate, MgClO4), if a permeation dryer is not used.6.2 Nitrogen-free solvent (e.g. toluene, isooctane or cetane), that produces a signal in the cas
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