Analytical Test Procedures of Specialty Silica

Determination Determination of Total Silicon Dioxide Content in Silicas

0130 According to the Test Procedure 0130 E.04 ccording 3262Following ISO 3262-19 1. Purpose

This testing method is used for the gravimetrical determination of the total silicon dioxide content of silica, after-treated silica and aluminum silicate. 2. ISO LOI PA Abbrevia Terms and Abbreviations International Organization for Standardization Loss on ignition Testing method

LOD Loss on drying

SAP Systems applications and products in data processing 3. 3.1 Descrip Description Principle

The sample is repeatedly treated with hydrochloric acid and evaporated to dryness. To render dehydrated silicon dioxide thus formed as insoluble as possible, it is heated for 2 hours at (140 5) C. Any chlorides present are removed by extracting the precipitate with hot dilute hydrochloric acid. The precipitate is ignited at 1000 C and treated with hydrofluoric and sulfuric acid. The silicon dioxide is evaporated off as silicon tetrafluoride. The mass loss after the evaporation is conform to the silicon dioxide content of the sample. 3.2 Equipment

Use ordinary laboratory apparatus and glassware, together with the following: 3.2.1 Analytical balance with an accuracy of 0.1 mg 3.2.2 Platinum crucible 3.2.3 Dish 3.2.4 Water bath, capable of being maintained at 100 C 3.2.5 Infrared evaporator (or other similar equipment) 3.2.6 Drying oven, capable of beeing maintained at (140 5) C
IM-SI-PS-AT, Silica-Analytics Dr. Udo Grl udo.goerl@evonik.com

3.2.7 Muffle furnace, capable of beeing maintained at (1000 20) C 3.2.8 Desiccator, containing magnesium perchlorate as desiccant 3.2.9 Filter paper (The filter paper used for filtration of the silicon dioxide shall be of such texture as to retain the smallest particles of precipitate and nevertheless permit rapid filtration. (e.g. Whatman No. 40 or 41, Schleicher und Schll No. 589/2 "Weiband")

3.3

Reagents

Use only reagents of recognized analytical grade. 3.3.1 De-ionized or distilled water 3.3.2 Hydrochloric acid, concentrated, approximately 32 % (m/m) 3.3.3 Hydrochloric acid, diluted 1 + 1 (Add 1 part by volume of concentrated hydrochloric acid (3.3.2) to 1 part by volume of de-ionized water) 3.3.4 Sulfuric acid, diluted 1 + 1 (Add 1 part by volume of concentrated sulfuric acid, approximately 96 % (m/m) slowly to 1 part by volume of de-ionized water) 3.3.5 Hydrofluoric acid, concentrated, approximately 40 % (m/m) 3.4 3.4.1 3.4.1.1 Testing Procedure Operating Procedure Gravimetrical determination of the silicon dioxide content

1g (m0) of the sample is weighed to the nearest 0.2 mg in a dish (3.2.3) by means of an analytical balance. 20 ml of concentrated hydrochloric acid (3.3.2) are added slowly to the sample and evaporated to dryness under the infrared evaporator (3.2.5). 20 ml of concentrated hydrochloric acid are added again and evaporated to dryness. This step is repeated once more. After the third evaporation, the dish with the pre-treated sample is heated for 2 hours at (140 5) C by means of a drying oven (3.2.6). The dish is removed from the oven and allowed to cool down to ambient temperature. 50 ml of diluted 1 + 1 hydrochloric acid (3.3.3) are added to the residue in the dish and the suspension is warmed up to 100 C for approximately 20 minutes by means of a water bath (5.2.4). Afterwards the suspension is filtered through a suitable filter paper (5.2.9) and the residue on the filter is washed with hot water until the washings are neutral. The filtrate and washings are poured into the original dish and evaporated to dryness. This evaporation step is repeated another two times, adding each time 10 ml of concentrated hydrochloric acid to the residue. After the third evaporation, the dish with the residue is heated for 2 hours at (140 5) C by means of a drying oven. The dish is removed from the oven and allowed to cool down to ambient temperature. 20 ml of diluted 1 + 1 hydrochloric acid are added to the residue in the dish and the suspension is warmed up to 100 C for approximately 10 minutes by means of a water bath. Afterwards the suspension is filtered through a fresh filter paper and the residue on the filter is washed with hot water until the washings are neutral.
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If it is felt necessary, the filtrate is checked for any silicon which may have passed through the filter. The two filter papers with the washed precipitates are placed in a platinum crucible (5.2.2). After drying the filter papers with the residues, they must be ashed carefully at low temperature before igniting by means of a muffle furnace (3.2.7) at (1000 20) C to constant mass (this should take approximately 1 hour). After cooling down to ambient temperature in a desiccator (3.2.8), the ignited residue is weighed to the nearest 0.2 mg (m1) by means of an analytical balance. The ignited residue in the platinum crucible is wetted with 2 - 3 ml of de-ionized water, added 1ml of diluted 1 + 1 sulfuric acid (3.3.4) and 15 ml of concentrated hydrofluoric acid (3.3.5) and evaporated to a syrup under taking care to avoid loss by spitting. After cooling down to ambient temperature, adhearend particles on the wall of the platinum crucible are rinsed into the syrup by using small quantities of water. A further 10 ml of concentrated hydrofluoric acid are added and evaporated to dryness. If the evaporation of the silicon tetrafluoride is not complete, a further 10 ml of concentrated hydrofluoric acid are added and evaporated to dryness again. The residue is heated until white fumes are no longer evolved and ignited for 30 minutes at (1000 20) C by means of a muffle furnace. After cooling down to ambient temperature in a desiccator, the ignited residue is weighed to the nearest 0.2 mg (m2) by means of an analytical balance. 3.4.1.2 Determination of the total loss on ignition

The total loss on ignition (LOI) is determined at 1000C for 2 hours according to testing method PA 0550 (following ISO 3262-1). 3.4.1.3 Determination of the total loss on drying

The total loss on drying (LOD) is determined at 105C for 2 hours according to testing method PA 0040 (following ISO 787-2). 3.4.2 3.4.2.1 Evaluation Evaluation of the total silicon dioxide content based on original substance

wSiO2 =

(m1 m2 ) 100
m0

With: wSiO2 m0 m1 m2
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: mass fraction of total silicon dioxide based on original substance [%] : mass of weighed sample [g] : mass of dehydrated silicon dioxide after treatment with hydrochloric acid and ignition at (1000 20) C to constant mass (see 3.4.1.1) [g] : mass of silicon dioxide after treatment with hydrofluoric acid and
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ignition at (1000 20) C to constant mass (see 3.4.1.1) [g] 3.4.2.2 Evaluation of the total silicon dioxide content based on ignited substance

wSiO2 ignited =

w SiO2 100 100 - LOI

With: wSiO2 ignited wSiO2 LOI : mass fraction of total silicon dioxide based on ignited substance [%] : mass fraction of total silicon dioxide based on original substance [%] : loss on ignition, 2h/1000C (based on original substance) [%] (see 3.4.1.2)

3.4.2.3

Evaluation of the total silicon dioxide content based on dried substance

wSiO2 dried =

w SiO2 100 100 - LOD

With: wSiO2 dried wSiO2 LOD : mass fraction of total silicon dioxide based on dried substance [%] : mass fraction of total silicon dioxide based on original substance [%] : loss on drying (2h, 105C) (see 3.4.1.3) [%]

The total silicon dioxide content is determined by repeated testing. The mean of the repeated testing is calculated and the result is reported to the nearest 0.1 %. 4. 4.1 Indications and Remarks Reference Documents

ISO 3262-19 4.2 Validation of the Procedure

The method is validated as an ISO procedure. 4.3 Safety Instructions

This testing procedure requires handling with chemicals and hot laboratory equipment. Therefore the safety guidelines for the use of sulfuric acid, and hydrofluoric acid are to be considered.

IM-SI-PS-AT, Silica-Analytics Dr. Udo Grl udo.goerl@evonik.com

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The "guidelines for laboratories of the professional association of the chemical industry" apply to work in chemical laboratories in general and, therefore, should be kept in mind. 4.5 Reference for SAP-Spezial

SAP inspection characteristics for quality field 645: Property K119 (SiO2 content based on ignited substance, %) K120 (SiO2 content based on dried substance, %) K121 (SiO2 content based on original substance, %) Test Method K044

IM-SI-PS-AT, Silica-Analytics Dr. Udo Grl udo.goerl@evonik.com

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