SIST-TS CEN/TS 16375:2013

Liming materials - Determination of the amount of residual finely ground carbonate in soils - Volumetric method

This Technical Specification specifies a method for the determination of low contents (as < 5 g CaCO3 per kilogram) of carbonate in soil samples. It applies to any type of carbonate liming material, such as limestone, chalk, and dolomite.

Calcium-/Magnesium-Bodenverbesserungsmittel - Bestimmung der Menge feingemahlener Carbonatrückstände in Böden - Volumetrisches Verfahren

Diese Technische Spezifikation legt ein Verfahren zur Bestimmung von geringen Gehalten (wie z. B.  5 g CaCO3 je Kilogramm) an Carbonat in Bodenproben fest. Das Verfahren gilt für alle Arten von carbonatischen Calcium-/Magnesium-Bodenverbesserungsmitteln, wie z. B. Kalkstein, Kreide und Dolomit.

Amendements minéraux basiques - Détermination de la teneur en carbonate résiduel finement broyé dans les sols - Méthode volumétrique

Le présent document spécifie une méthode de détermination des faibles teneurs ( 5 g CaCO3 par kilogramme) en carbonate dans les échantillons de sols. Il s’applique à tout type d’amendement minéral basique carbonaté, comme le calcaire, la craie, la dolomie.

Sredstva za apnjenje - Določevanje količine preostalih fino mletih karbonatov v tleh - Volumetrijska metoda

Ta tehnična specifikacija določa metodo za določevanje nizkih vsebnosti (kot je < 5 g CaCO3 na kilogram) karbonatov v vzorcih tal. Uporablja se za vse vrste karbonatnega sredstva za apnenje, kot so apnenec, kreda in dolomit.

General Information

• Status: Published
• Public Enquiry End Date: 09-Apr-2012
• Publication Date: 21-Apr-2013
• ICS: 65.080 - Fertilizers
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 04-Apr-2013
• Due Date: 09-Jun-2013
• Completion Date: 22-Apr-2013
• Ref Project: CEN/TS 16375:2013 - Liming materials - Determination of the amount of residual finely ground carbonate in soils - Volumetric method

Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN/TS 16375:2013
01-maj-2013
6UHGVWYD]DDSQMHQMH'RORþHYDQMHNROLþLQHSUHRVWDOLKILQRPOHWLKNDUERQDWRYY
WOHK9ROXPHWULMVNDPHWRGD
Liming materials - Determination of the amount of residual finely ground carbonate in
soils - Volumetric method
Calcium-/Magnesium-Bodenverbesserungsmittel - Bestimmung der Menge
feingemahlener Carbonatrückstände in Böden - Volumetrisches Verfahren
Amendements minéraux basiques - Détermination de la teneur en carbonate résiduel
finement broyé dans les sols - Méthode volumétrique
Ta slovenski standard je istoveten z: CEN/TS 16375:2013
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 16375:2013 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 16375:2013

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SIST-TS CEN/TS 16375:2013


TECHNICAL SPECIFICATION
CEN/TS 16375

SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION
January 2013
ICS 65.080
English Version
Liming materials - Determination of the amount of residual finely
ground carbonate in soils - Volumetric method
Amendements minéraux basiques - Détermination de la Calcium-/Magnesium-Bodenverbesserungsmittel -
teneur en carbonate résiduel finement broyé dans les sols - Bestimmung der Menge feingemahlener
Méthode volumétrique Carbonatrückstände in Böden - Volumetrisches Verfahren
This Technical Specification (CEN/TS) was approved by CEN on 27 May 2012 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16375:2013: E
worldwide for CEN national Members.

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Contents Page
Foreword . 3
1 Scope . 4
2 Normative references . 4
3 Principle. 4
4 Reagents . 4
5 Apparatus . 4
6 Procedure . 7
6.1 Preparation of the apparatus . 7
6.2 Sample preparation . 8
6.3 Measurement procedure . 8
7 Method by controlled additions . 9
7.1 General . 9
7.2 Procedure . 9
7.3 Calculation and expression of the results . 9
8 Method by direct measurement . 10
8.1 General . 10
8.2 Choice of a pilot soil without carbonate . 10
8.3 Calibration of the calcimeter. 10
8.3.1 Procedure . 10
8.3.2 Calculation and expression of the result . 10
8.4 Measurement of an unknown sample . 11
8.4.1 Procedure . 11
8.4.2 Calculation and expression of the results . 11
9 Precision . 11
9.1 Inter-laboratory test . 11
9.2 Repeatability . 12
9.3 Reproducibility . 12
10 Test report . 13
Annex A (informative) Using spread sheet software to calculate linear regression . 14
Bibliography. 15

2

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Foreword
This document (CEN/TS 16375:2013) has been prepared by Technical Committee CEN/TC 260 “Fertilizers
and liming materials”, the secretariat of which is held by DIN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
3

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1 Scope
This Technical Specification specifies a method for the determination of low contents (as < 5 g CaCO per
3
kilogram) of carbonate in soil samples. It applies to any type of carbonate liming material, such as limestone,
chalk, and dolomite.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this 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.
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)
3 Principle
Hydrochloric acid is added to a soil sample to decompose any carbonates present. The reaction in simplified
form reads as follows (Me means metal):
+ 2+

MeCO + 2H → Me + H CO
3 2 3
H CO → H O+ CO (gaseous)
2 3 2 2
The volume of the carbon dioxide produced is measured with a measuring burette, and is compared with the
volume of gas produced by increasing amounts of calcium carbonate added to test portions. To avoid making
corrections for differences in temperature and pressure, all determinations are carried out under the same
conditions, with a very strict control of ambient conditions and determination timing, e.g. air-conditioned room
and water bath, short time during which the variation of atmospheric pressure is supposed to be constant.
4 Reagents
Use only reagents of recognized analytical grade.
4.1 Water, with a specific electrical conductivity not higher than 0,2 mS/m at 25 °C (conforming to grade 2
of EN ISO 3696).
4.2 Hydrochloric acid, c(HCl) = 4 mol/l.
Dilute 340 ml of 37 % hydrochloric acid in water (4.1) and then fill up to 1 000 ml with water (4.1).
4.3 Sulfuric acid, (H SO ) solution 95 % to 97 %.
2 4
4.4 Sodium sulfate, (Na SO ), powder, purity higher than 99 %.
2 4
4.5 Internal liquid of the calcimeter, 50 g/l of sodium sulfate (4.4) and 50 ml/l of sulfuric acid (4.3).
4.6 Calcium carbonate, (CaCO ), powder, purity higher than 99 %.
3
5 Apparatus
5.1 Apparatus for the volumetric measurement of produced gas, inspired of Bernard calcimeter
according to Figure 1.
The apparatus is composed of a glass tube of 20 ml graduated every 0,02 ml. The total length shall not
exceed 80 cm. Another non graduated glass tube with the same length and the same diameter is connected
to the first glass tube with a transparent flexible pipe of about 1 m. A small volume of reserve of 50 ml can be
inserted right at the inferior end of the graduated tube. The higher end of the graduated tube is connected by a
standard flexible pipe to the Erlenmeyer flask (5.2) of attack.
4

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The graduated tube is fixed vertically on a stand.
The non-graduated tube is held on a second stand, parallel to the first, but so that it is vertically mobile. Mark
the tube to approximately 2 cm of its lower end.
The two tubes shall only be 1 mm or 2 mm away from each other.
The whole apparatus shall be dipped several hours in a surface-active cleaning liquid to eliminate any trace
on the interior surface of the tubes which could hinder circulation and modify the levelling of the internal liquid.
Rinse with demineralised water after treatment.
5

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Key
A glass tube of 20 ml graduated every 0,02 ml
B non-graduated tube
C flexible pipe
C’ standard flexible pipe
D bulb of 50 ml
E 200 ml Erlenmeyer flask with finely ground, gas tight glass stopper
F water bath
L metallic ring
R 3 ways tap
S stand
T reaction tube (with hydrochloric acid)
Figure 1 — Calcimeter
5.2 200 ml Erlenmeyer flask, with finely ground, gas tight glass stopper.
Erlenmeyer flasks of attack, with a capacity of 200 ml, are closed by a finely ground glass cup. The upper part
of the cap is connected by 200 mm of standard flexible pipe to a 3 ways tap of polytetrafluoroethylene, PTFE),
which is also connected to the flexible pipe coming from the graduated tube.
The waterproof of the glass cap is ensured by a thin silicone-grease layer.

5.3 Water bath, the volume of water shall be of at least 5 l and maintain at room temperature.
6

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5.4 Metallic ring.
The Erlenmeyer flask of attack (5.2) is ballasted with a metallic ring and is kept in the water bath.
5.5 Thermo stated room.
The whole device is placed in a thermo stated room of a great thermal inertia or fit with a device of cold-hot
regulation which ensures an uninterrupted constant temperature to ± 1 °C. Check the room temperature
changes close to the device for 1 h.
The analysis may only start wh
...