SIST EN 13466-1:2002

SIST EN 13466-1:2002 is the Slovenian adoption of EN 13466-1:2001 from CEN. It specifies a Karl Fischer titrimetric method for determining water content in solid mineral fertilizers using methanol as the extracting medium, for laboratories and quality-control teams that need a comparable result for product assessment, storage and handling.

What does SIST EN 13466-1:2002 specify?

SIST EN 13466-1:2002 covers one laboratory method in the EN 13466 series: Part 1 uses methanol as the extracting medium. The method is written for all solid mineral fertilizers and reports a result called KFM water.

The scope matters because the reported water content is not just free water. It also includes extracted water of crystallization from listed fertilizer components, and it notes that methanol-soluble metal oxides and hydroxides can affect the result if their content is known.

The document is organized into:

• Scope
• Normative references
• Principle
• Reagents
• Apparatus
• Installation and test of the Karl Fischer titrator
• Sampling
• Procedure
• Calculation and expression of results
• Precision
• Test report

What are the key requirements of SIST EN 13466-1:2002?

Sample type and result meaning

SIST EN 13466-1:2002 is intended for solid mineral fertilizers. In practice, that means the method fits routine control of granular or powder fertilizers, not liquid products or other material types.

The result, KFM water, includes free water and water released from specified crystalline components. For users, this is important when comparing products that contain hydrates, because the method can read some bound water as part of the measured moisture.

Reagents and equipment

SIST EN 13466-1:2002 requires analytical-grade reagents, methanol with very low water content, a Karl Fischer reagent with a stated water equivalence, sodium tartrate dihydrate for calibration, and ordinary laboratory glassware plus a balance readable to 0.0001 g.

That equipment list shows the method is a precise titrimetric test. In practice, labs need good weighing accuracy, controlled reagent quality, and a titrator that can detect the equivalence point reliably.

Titrator setup, calibration and drift

SIST EN 13466-1:2002 requires the Karl Fischer titrator to be installed and checked according to the manufacturer’s instructions. The reagent is standardized with a known amount of water or with sodium tartrate dihydrate, and drift from atmospheric moisture must be measured and taken into account.

This matters because water can enter the titration cell from the air. If a laboratory does not correct for drift, the reported water content can be biased high.

How the determination is performed

SIST EN 13466-1:2002 uses two practical routes. If the fertilizer disperses or dissolves in methanol, the test portion is added directly to methanol in the titration vessel. If it does not, the sample is extracted in methanol in a centrifuge tube, dispersed with a high-speed dispersing device, centrifuged, and only the clear supernatant is titrated.

The method also sets test-portion masses according to expected water content and reagent titre, and it limits dispersion temperature, especially for fertilizers containing magnesium sulfate. In practice, the analyst has to choose the right preparation route and avoid heating the sample enough to change its water release behavior.

Blank test, repeat test and reporting

SIST EN 13466-1:2002 requires a blank test carried out by the same procedure without sample, and it requires a second determination on another test portion. The final result is the mean of two determinations, corrected for blank and drift.

The test report must identify the sample, state the method used, describe sampling and sample preparation, give the result as mass fraction wKFM water = x %, and note any unusual features. That makes the result traceable for quality records, disputes and purchasing checks.

What terms does SIST EN 13466-1:2002 define?

• KFM water - The reported water content from this methanol-based Karl Fischer method, including free water and certain extracted waters of crystallization.
• Karl Fischer reagent - The titrant used to react specifically with water during the determination.
• Equivalence point - The endpoint at which the amount of reagent added matches the water present in the test solution.
• Drift - Water entering the titration system from the air during the test, which must be measured and corrected for.
• CAN - Calcium ammonium nitrate, named in the procedure as a fertilizer that is usually dispersible in methanol.
• Test portion - The weighed amount of sample actually used in one determination.
• Blank test - A run through the same steps without sample, used to correct the result for background water.

Who uses SIST EN 13466-1:2002?

SIST EN 13466-1:2002 is used by fertilizer testing laboratories, production quality-control teams, contract laboratories and inspection bodies working with solid mineral fertilizers. They use it to measure moisture for product release, incoming inspection, stability checks and handling decisions.

It is especially relevant where water content affects storage behavior, caking risk or the interpretation of hydrate-containing fertilizers. Buyers and specifiers can also use it to compare laboratory results on the same technical basis.

What changed in SIST EN 13466-1:2002 from the previous edition?

SIST EN 13466-1:2002 is identified as identical to EN 13466-1:2001.

Which standards are used with SIST EN 13466-1:2002?

• EN 1482 - Gives the sampling method for solid fertilizers and liming materials, which this standard uses for taking the test sample.
• EN 13466-2 - The companion part of the EN 13466 series, covering 2-propanol as the extracting medium.
• EN 12048 - Cited in the introduction as a gravimetric moisture method with limited applicability.
• EN 12049 - Cited in the introduction as another gravimetric moisture method with limited applicability.

What does the SIST EN 13466-1:2002 document contain?

SIST EN 13466-1:2002 contains a full laboratory procedure, from sampling and reagent preparation through direct titration or methanol extraction and centrifugation. Tables 1 and 2 set the test-portion masses according to expected water content and reagent titre.

Clause 9 gives the calculation basis, including correction for blank and drift, and clause 10 gives repeatability and reproducibility from an interlaboratory study. Clause 11 specifies what the test report must include. The bibliography points to related moisture standards and to the precision study used to support the method.