DIN ISO 11916-1-2014 Soil quality - Determination of selected explosives and related compounds - Part 1 Method using high-performance liquid chromatography (HPLC) with ultraviolet .pdf

1、November 2014 Translation by DIN-Sprachendienst.English price group 14No 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).I

2、CS 13.080.10!%=cE“2266434www.din.deDDIN ISO 11916-1Soil quality Determination of selected explosives and related compounds Part 1: Method using high-performance liquid chromatography (HPLC)with ultraviolet detection (ISO 11916-1:2013),English translation of DIN ISO 11916-1:2014-11Bodenbeschaffenheit

3、 Bestimmung von ausgewhlten Explosivstoffen und verwandten Verbindungen Teil 1: Verfahren mittels Hochleistungs-Flssigkeitschromatographie (HPLC) undUV-Detektion (ISO 11916-1:2013),Englische bersetzung von DIN ISO 11916-1:2014-11Qualit du sol Dosage dune slection dexplosifs et de composs apparents P

4、artie 1: Mthode utilisant la chromatographie liquide haute performance (CLHP) avecdtection ultraviolet (ISO 11916-1:2013),Traduction anglaise de DIN ISO 11916-1:2014-11www.beuth.deDocument comprises 29 pagesIn case of doubt, the German-language original shall be considered authoritative.10.14 Conten

5、ts PageNational foreword .21 Scope . 52 Normative references 53 Principle 64 Interferences 65 Reagents 65.1 General . 65.2 Chemicals . 65.3 Standard substances and solutions . 76 Apparatus . 76.1 General . 76.2 Equipment for extraction . 86.3 High-performance liquid chromatography (HPLC) system with

6、 DAD 87 Procedure. 87.1 Sample pretreatment, sample storage and determination of water content 87.2 Extraction 97.3 Storage of extract . 118 High-performance liquid chromatographic analysis 118.1 General 118.2 High-performance liquid chromatographic system . 118.3 Calibration . 128.4 Identification

7、and quantification 139 Calculation of results 1310 Quality assurance . 1311 Expression of results .1412 Test report 14Annex A (informative) Method-checking standard recovery limit 15Annex B (informative) HPLC-UV-DAD conditions .16Annex C (informative) Precision data .20Bibliography .29A comma is use

8、d as the decimal marker. DIN ISO 11916-1:2014-11 2National Annex NA (informative) Bibliography 3National foreword This document (ISO 11916-1:2013) has been prepared by Technical Committee ISO/TC 190 “Soil quality” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparati

9、on was the DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Group NA 119-01-02-02-53 AK Sprengstofftypische Verbindungen of Working Committee NA 119-01-02 AA Boden- und Abfalluntersuchung. Attention is drawn to the possibility that some of the elements of this docume

10、nt may be the subject of patent rights. DIN shall not be held responsible for identifying any or all such patent rights. ISO 11916 consists of the following parts, under the general title Soil quality Determination of selected explosives and related compounds: Part 1: Method using high-performance l

11、iquid chromatography (HPLC) with ultraviolet detection Part 2: Method using gas chromatography (GC) with electron capture detection (ECD) or mass spectrometric detection (MS) As a result of national implementation in Germany, the following should be noted: A shaking width of about 10 cm of the horiz

12、ontal mechanical shaker as given in Subclause 6.2.2 is not realistic. Conventional horizontal mechanical shakers are preset according to type and are not adjustable. Experience has shown that shaking widths between 5 cm and 7 cm are adequate. The DIN Standards corresponding to the International Stan

13、dards referred to in this document are as follows: ISO 565 DIN ISO 565 ISO 5725-2 DIN ISO 5725-2 ISO 11465 DIN EN 15934 ISO 11916-2 DIN ISO 11916-2 ISO 14507 DIN 19747 ISO 22478 DIN EN ISO 22478 WARNING Users of this Standard should be familiar with normal laboratory practice. This standard does not

14、 purport to address all the safety aspects, if any, associated with its use. It is the responsibility of the employer to establish appropriate safety and protective practices and to ensure compliance with any national regulatory conditions. IMPORTANT Expert assistance and specialized laboratories wi

15、ll be required to perform the analyses described in this standard. DIN ISO 11916-1:2014-11 3 National Annex NA (informative) Bibliography DIN 19747, Investigation of solids Pretreatment, preparation and processing of samples for chemical, biological and physical investigations DIN EN 15934, Sludge,

16、treated biowaste, soil and waste Calculation of dry matter fraction after determination of dry residue or water content DIN EN ISO 22478, Water quality Determination of certain explosives and related compounds Method using high-performance liquid chromatography (HPLC) with UV detection DIN ISO 565,

17、Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method

18、 DIN ISO 11916-2, Soil quality Determination of selected explosives and related compounds Part 2: Method using gas chromatography (GC) with electron capture detection (ECD) or mass spectrometric detection (MS) DIN ISO 11916-1:2014-11 4 Soil quality Determination of selected explosives and related co

19、mpounds Part 1: Method using high-performance liquid chromatography (HPLC) with ultraviolet detection1 ScopeThis part of ISO 11916 specifies the measurement of explosive and related nitrocompounds (as given in Table 1) in soils and soil materials. This part of ISO 11916 is intended for the trace ana

20、lysis of explosives and related compounds by high-performance liquid chromatography (HPLC) using an ultraviolet (UV) detector.Under the conditions specified in this part of ISO 11916, concentrations as low as 0,1 mg/kg to 1 mg/kg dry matter can be determined, depending on the substance. Similar comp

21、ounds, in particular various nitroaromatics, by-products and degradation products of explosive compounds may be analysed using this method. However, the applicability should be checked on a case-by-case basis.Table 1 Explosive and related nitrocompounds for analysisCompound Abbreviation CAS-RNaNitro

22、benzene NB 98-95-31,3-Dinitrobenzene 1,3-DNB 99-65-01,3,5-Trinitrobenzeneb1,3,5-TNB 99-35-42-Nitrotoluene 2-NT 88-72-23-Nitrotoluene 3-NT 99-08-14-Nitrotoluene 4-NT 99-99-02,4-Dinitrotoluene 2,4-DNT 121-14-22,6-Dinitrotoluene 2,6-DNT 606-20-22,4,6-Trinitrotoluene 2,4,6-TNT 118-96-74-Amino-2,6-dinitr

23、otoluene 4-A-2,6-DNT 19406-51-62-Amino-4,6-dinitrotoluene 2-A-4,6-DNT 35572-78-2N-Methyl-N-2,4,6-tetranitroanilinebTetryl 479-45-82,4,6-Trinitro-N-(2,4,6-trinitrophenyl)aniline Hexyl 131-73-71,3,5-Trinitrohexahydro-1,3,5-triazine RDX 121-82-41,3,5,7-Tetranitrooctahydro-1,3,5,7-tetrazocine HMX 2691-4

24、1-0PentaerythrityltetranitratebPETN 78-11-5aCAS-RN: Chemical Abstract Service-Registry NumberbPETN, 1,3,5-TNB and tetryl gave poor interlaboratory trial results and their analysis could be problematic2 Normative referencesThe following documents, in whole or in part, are normatively referenced in th

25、is document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.DIN ISO 11916-1:2014-11 5 ISO 565, Test sieves Metal wire cloth, perforated metal plat

26、e and electroformed sheet Nominal sizes of openingsISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric methodISO 22478, Water quality Determination of certain explosives and related compounds Method using high-performance liquid chromatography (HPLC) wit

27、h UV detection3 PrincipleExplosive materials in soils are extracted with acetonitrile or methanol, using one of the following techniques: ultrasonic bath with ultrasonic waves as medium (USE); horizontal mechanical shaker at room temperature (MSE); Soxhlet apparatus that works isothermically at boil

28、ing temperature (SOX); pressurized liquid extraction (PLE).The extract containing the analytes is either injected directly, or if necessary diluted prior to injection, into a reversed-phase high-performance liquid chromatography system (HPLC) and the analytes are detected by means of a diode array d

29、etector (DAD).WARNING Take care when transporting, storing or treating explosive materials. High temperature, high pressure and static electricity shall be prevented when storing explosive materials. Small amounts of explosive materials should be kept moist in a cool, dark place. Soil samples contai

30、ning explosives with a mass fraction of less than 1 % do not have a risk of explosion.4 InterferencesSolvents, reagents, glassware, and other hardware used for sample processing may yield artefacts and/or elevated baselines, causing misinterpretation of the chromatograms. All of these materials shal

31、l therefore be demonstrated to be free of contaminants and interferences through the analysis of method blanks.Tetryl may decompose in methanol or water at (or above) room temperature. Degradation products of tetryl appear as a shoulder of 2,4,6-TNT when a C18column is used. In this case, evaluation

32、 of 2,4,6-TNT should be based on peak height rather than peak area.Samples containing 2,4,6-trinitrobenzoic acid should not be extracted with acetonitrile as it may result in the overestimation of 1,3,5-TNB, due to decarboxylation.5 Reagents5.1 GeneralAll reagents shall be blank-free and of recogniz

33、ed analytical grade. They shall not contain any measurable quantities of UV-absorbing substances that may interfere with the determination.5.2 Chemicals5.2.1 Water.5.2.2 Acetone, C3H6O, for the cleaning of containers and devices.5.2.3 Acetonitrile, CH3CN, HPLC grade or equivalent.DIN ISO 11916-1:201

34、4-11 6 5.2.4 Methanol, CH3OH, HPLC grade or equivalent.5.2.5 Diatomaceous earth or sea sand, pelletized and calcinated (for PLE).5.3 Standard substances and solutions5.3.1 Standard substances5.3.1.1 Reference substancesCompounds listed in Table 1.5.3.1.2 Method-checking standardSuitable compound(s)

35、not found in the sample, e.g. 2,5-DNT.5.3.2 Standard solutions5.3.2.1 GeneralAll standard solutions used in this method shall be prepared as described below.NOTE If commercially available certified standard stock solutions (Table 1) are used, calibration solutions are prepared in volumetric flasks b

36、y diluting the stock solutions with acetonitrile (5.2.3) or methanol (5.2.4), respectively.All dilution steps shall not exceed the factor 100.5.3.2.2 Single-substance stock solutionsFor the preparation, weigh 50 mg 0,1 mg of the reference substances into 50 ml measuring flasks (scale: mg/ml), fill u

37、p to the mark with acetonitrile (5.2.3) or methanol (5.2.4), respectively and let them dissolve completely.Transfer the stock solutions to amber-glass flasks and seal with PTFE-coated screw caps.The stock solutions can be kept in the refrigerator at 2 C to 6 C in the dark for up to 1 year.5.3.2.3 Mu

38、lti-component stock solutionsPrepare multi-component stock solutions of different concentrations from the various single-substance stock solutions (5.3.2.2) by mixing and diluting with acetonitrile (5.2.3) or methanol (5.2.4), respectively.At concentrations below 1 mg/ml, solutions should be checked

39、 after one week as reference substances may decompose.For calibration standards, a minimum of 5 concentration levels is needed.6 Apparatus6.1 GeneralUsual laboratory apparatus and the following.6.1.1 Amber glass containers with caps containing polytetrafluoroethene (PTFE) coated lining.6.1.2 Amber g

40、lass vials with caps containing septa with polytetrafluorethene (PTFE) coated lining.7DIN ISO 11916-1:2014-11 6.1.3 Amber glass conical bottles with ground-in stopper.6.1.4 Perforated metal plate sieve, complying with ISO 565.6.1.5 Analytical balance, with a precision of at least 0,1 mg.6.1.6 Labora

41、tory centrifuge, capable of producing an acceleration of at least 1 000g.6.1.7 pH-meter, to adjust the pH of the mobile phase for HPLC.6.1.8 Filter and suitable filter discs, 0,45 m pore size.Any adsorption of the target analytes shall be avoided. No interfering material shall be eluated. PTFE or po

42、lyamide material is recommended.6.2 Equipment for extraction6.2.1 Temperature-controlled ultrasonic bath, 35 Hz, effective HF-power of at least 140 W.Water bath capable of maintaining the temperature at (30 5) C or at (50 5) C during ultrasonic extraction.6.2.2 Horizontal mechanical shakerThe shaker

43、 shall maintain a frequency of 100 cycles/min and offer a shaking width of about 10 cm.6.2.3 Soxhlet apparatusExtractor, whose extraction chamber and syphon are placed inside the steam chamber and suitably covered, or extractor with additionally heated extraction chamber, complete with boiling vesse

44、l, suitable heating mantle and reflux condenser, suitable for the extraction of a 50 g sample of soil with a hot solvent distillate through complete flooding of the extractive.6.2.4 Pressurized liquid extractor (PLE)Pressurized liquid extraction device, equipped with extraction cells made of stainle

45、ss steel or other material capable of withstanding the pressure levels (890 hPa/2 000 psi) necessary for this procedure; vials for collection of extracts, 40 ml or 60 ml, pre-cleaned, open-top screw-cap with polytetrafluoroethylene (PTFE)-lined septum; filter disc, cellulose or glass fibre; cell cap

46、 sealing disc.6.3 High-performance liquid chromatography (HPLC) system with DADHPLC system, consisting of a pump which supports a pressure of at least 40 MPa (400 bar), an injection system with a loop capacity of 100 l and a diode array detector (DAD) with wavelength range of 200 nm to 400 nm (or hi

47、gher).Other specifications of the HPLC system should be in accordance with ISO 22478.7 Procedure7.1 Sample pretreatment, sample storage and determination of water contentWhile taking a field-moist sample, remove coarse impurities, e.g. plant residues and stones. Put the sample in an amber glass flask and store immediately in a cool, dark transport container.Soil samples shall be analysed as soon as possible.DIN ISO 11916-1:2014-11 8