ISO/DIS 1014-2:2024(en)

ISO TC 27/SC 3/WG 1

Secretariat: SABS

Date: 2024-09-04

Coke — Determination of true relative density

© ISO 2024

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Contents

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7 Procedure Error! Bookmark not defined.

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10 Test report Error! Bookmark not defined.

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Foreword

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This document was prepared by Technical Committee ISO/TC 27, Coal and coke, Subcommittee SC 3, Coke.

This is the first edition of this document and was created to separate ISO 1014:2021 into three separate documents in accordance with a resolution passed during the 16th Plenary Meeting of ISO TC27 SC3 17 May 2023 in Delft, The Netherlands.

A list of all parts in the ISO 1014 series can be found on the ISO website.

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Coke — Determination of true relative density

This document specifies the method for determining the true relative density of coke, in relation to water.

NOTE “True relative density” varies according to the displacement liquid used.

The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 3310‑2, Test sieves — Technical requirements and testing — Part 2: Test sieves of perforated metal plate

ISO 13909‑6, Coal and coke — Mechanical sampling — Part 6: Coke — Preparation of test samples

ISO 18283, Coal and coke — Manual sampling

No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https://www.iso.org/obp

— IEC Electropedia: available at https://www.electropedia.org/

The mass of water displaced by a known mass of dry coke, ground to pass through a 212 µm sieve, is determined using a pycnometer. Air is displaced by boiling during the determination. Distilled water is specified. Thermostatic control of the temperature is essential since a difference of 1 °C can cause an error of about 0,012 in the result.

5.1 Pycnometer, 50 ml capacity, Figure 1.

5.2 Water bath, with stirrer, thermostatically controlled to maintain a desired temperature Ɵ °C to within ±1 °C.

5.3 Two wash bottles, each containing about 50 ml of distilled water. One wash bottle is kept hot (80 °C to 90 °C) and the other is left in the water bath (5.2).

5.4 Reflux air condenser: a glass tube about 1 m long, of the same external diameter as the neck of the pycnometer (5.1) with a short length of rubber tubing for attaching it to the latter.

5.5 Glycerol bath: a suitable vessel in which sufficient glycerol can be heated for the lower two-thirds of the pycnometer (5.1) to be immersed.

5.6 Analytical Balance, with a resolution of at least 0,1 % relative of the test portion mass.

Key

Figure 1 — Examples of pycnometers

The coke used for the determination is the general analysis sample, prepared to a nominal top size of 212 µm (see ISO 13909‑6 and ISO 18283). Before commencing the determination, mix the sample thoroughly for at least 1 min, preferably by mechanical means.

7.1 Clean the pycnometer (5.1), fill with distilled water. Insert the stopper and immerse the pycnometer up to the neck in the water bath (5.2) at Ɵ °C for 1 h. The value of Ɵ should be about 5 °C above the ambient temperature. At the end of 1 h, remove the blob of water from the top of the stopper with a piece of filter paper, remove the pycnometer from the water bath, rapidly cool to approximately ambient temperature under cold running water, dry, allow to stand beside the balance (5.6) for 30 min and determine the mass of the pycnometer to the nearest 0,1 mg. Empty the pycnometer and dry the neck.

Clean the pycnometer (5.1) using suitable reagents like a mixture of hydrogen peroxide and sulfuric acid or commercially available surfactant mixtures. If necessary, the cleaning can be enhanced by using an ultrasonic bath. After the cleaning step rinse thoroughly and fill with distilled water.

7.2 Dry a portion of the coke sample for 1 h at 105 °C to 110 °C (see 7.3), cool to ambient temperature, then determine the mass of about 5 g of the dry coke to the nearest 0,1 mg and transfer it completely to the pycnometer. Wash down any coke adhering to the neck or side of the pycnometer with distilled water, making up the volume to about 25 ml.

Attach the air condenser (5.4) to the neck of the pycnometer with the rubber tubing and immerse the pycnometer in the glycerol bath (5.5). Heat the bath so that the water in the pycnometer begins to boil vigorously. Wash down any scum of coke with a few millilitres of the hot, distilled water at ambient temperature.

After the water has boiled for 30 min, remove the pycnometer from the glycerol bath, detach the air condenser and allow the pycnometer to cool. Fill the pycnometer with distilled water at Ɵ °C, insert the stopper and immerse the pycnometer up to the neck in the water bath at Ɵ °C for 1 h, compensating for any contraction of the liquid by the addition of distilled water and ensuring that air bubbles are not trapped, either below the stopper or in the capillary.

At the end of 1 h, remove the blob of water from the top of the stopper, remove the pycnometer from the water bath, cool, dry, allow to stand beside the balance for 30 min and determine the mass of the pycnometer as before.

7.3 Some reactive cokes are hygroscopic and with such materials it is permissible to omit the drying procedure. In this case, a moisture determination is carried out at the same time on a separate portion of the analysis sample (see ISO 687) and the mass of coke taken is corrected accordingly.

The true relative density of the coke (dimension one), ρ, is given by the following Formula (1):

(1)

where

The result, preferably the mean of duplicate determinations (see 9), shall be reported to the nearest 0,01.

The results of duplicate determinations, carried out at different times in the same laboratory by the same operator using the same apparatus on representative portions taken from the same analysis sample, shall not differ by more than 0,03.

The means of the results of duplicate determinations, carried out in two different laboratories on representative portions taken from the same analysis sample, shall not differ by more than 0,05.

The test report shall include the following information:

a) identification of the sample tested;

b) a reference to this document, i.e. ISO 1014-2:2024;

c) the date of determination;

d) the results and the method of expression used.

Bibliography

[1] ISO 687, Coke — Determination of moisture in the general analysis test sample