Matrix certified reference material of agricultural soil containing selected pesticides

The certified reference material of agricultural soil AN-ZP03 was prepared by spiking selected relevant organic compounds into the original natural matrix. Selected pesticides are certified.

Packing:

50 g of powder of the respective soil with a particle size of less than 100 μm in amber glass bottle. The sample is stabilized by radiation 25kGy.

Intended use:

This certified reference materials is intended primarily for use in realizing metrological traceability, validation of analytical methods and the transfer of property values to other materials of similar composition.

Recommended analytical methods for method dependent measurements:

Gas and liquid chromatography

Metrological traceability:

Metrological traceability is realized by using certified calibration standards solutions for the calibration of measurement methods used (direct traceability to SI unit) and/or by simultaneous analysis of a matrix CRM (RM) of similar composition.

Homogeneity and stability:

Homogeneity and short term stability has been demonstrated according to the ISO GUIDE 35. This CRM will be monitored for over the period of its validity.

Storing and instruction for use:

This CRM has to be stored in original bottle at -18°C (optimal is in a freezer). The materials should be analysed in the "as received" state and their dry weight should be determined on non-analysed aliquots oven-dried at 105°C till the constant weight. The material in the bottle must be rehomogenized before each use by mechanical shaking of the content for 1-2 minutes. The bottle should be opened a minimum of 2 minutes after rehomogenization in order to prevent an escape of fine powder particles from the bottle into the environment and their sedimentation.

Certified and indicative values and their uncertainties:

The certified and indicative values of selected pesticides are summarized in Table 1 and 2. The overall means evaluated have been given a status of certified and indicative values using the following criteria: data should be available from at least 5 and 3 accepted laboratory means should be available for calculation of the overall mean for certified and indicative value, respectively. At combined uncertainties presented, the contribution of uncertainty of characterization of a particular property value is dominant.

Table 1: Certified and indicative values of selected pesticides.

• Analytes: concentration [μg/kg] / uncertainty [μg/kg]
• Atrazine: 450 / 25
• Azoxystrobin: 281 / 18
• Carbendazim: 285 / 32
• Diflufenican: (595) / (82)
• Dimethenamid: (332) / (45)
• Epoxyconazole: 191 / 15
• Fenpropidin: (105) / (11)
• Chlorotoluron: (80.4) / (9.7)
• Chlorpyrifos: 353 / 22
• Linuron: 447 / 32
• Metamitron: 566 / 30
• Metazachlor: (775) / (88)
• Methoxyfenozide: (779) / (103)
• Metconazole: 270 / 14
• Pendimethalin: 186 / 12
• Pethoxamid: (294) / (53)
• Prochloraz: 195 / 14
• Spiroxamine: 490 / 46
• Tebuconazole: 814 / 66
• Terbuthylazine: 444 / 33

All values corrected to a dry mass at 105°C. Uncertainty – expanded combined uncertainty (k=2) () indicative value.

Table 2: Indicative values of selected organochlorine pesticides

• Analytes: concentration [μg/kg] / uncertainty [μg/kg]
• Gamma-BCH: 604 / 95
• Delta-BCH: 640 / 74
• 2,4-DDT: 286 / 33
• 4,4-DDT: 512 / 75
• Endrin: 423 / 36
• 4,4-DDD: 418 / 60

All values corrected to a dry mass at 105°C. Uncertainty – expanded combined uncertainty (k=2).

This CRM will be monitored for over the period of its validity. If substantive changes of reference values occur, Analytika®, spol. s r.o. will notify the purchaser.

Participated laboratories in material characterization and interlaboratory comparison:

• Analytika, spol. s r.o.
• Agroscope; Environmental Analytics; Zurich
• ALS Czech Republic s.r.o.
• ARISTOTLE UNIVERSITY OF THESSALONIKI; Department of Chemistry, Environmental Pollution Control Laboratory (EPCL)
• ARPAV; Servizio Laboratori Veneto EST; Venezia Mestre
• Benaki Phytopathological Institute; Department of Pesticides Control and Phytopharmacy, Laboratory of Chemical Control of Pesticides,
• Eurofins Environment Testing Finland Oy; LAHTI
• Institut National de la Recherche Agronomique; Laboratoire d´analysis des sols; Arras
• Institute of Environmental Assessment and Water Research; Barcelona
• LABAQUA, S.A.U; POL. IND. LAS ATALAYAS; ALICANTE
• MetropoliLab Oy; Helsinki
• RECETOX, Masaryk University; Brno
• UKZUZ Brno; NRL; Department of Residual Analyses
• University of Bern, Institute of Geography
• University of Bordeaux; Oceanic and Continental Environments and Paleoenvironments (LPTC)
• Wageningen Food Safety Research (WFSR)

Note:

Detailed information about the production, homogeneity testing and characterization of this CRM are described in the Certification report, which is available on request.