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DIN EN 196

水泥试验方法 水泥中氯化物、二氧化碳和碱含量的测定

DIN EN 196

Methods of testing cement - Determination of the chloride, carbon dioxide and alkali content of cement

版本年份 1989 文件语言 英语 全文 6 页 格式 PDF
DIN EN 196 水泥试验方法 水泥中氯化物、二氧化碳和碱含量的测定封面

标准信息

STANDARD INFORMATION
标准编号
DIN EN 196
所属分类
DIN 德国标准
发布机构
CEN
版本年份
1989
文件语言
英语
文件格式
PDF
文件页数
6 页
文件大小
485.23 KB

中文名称为参考译名,文件语言以原文为准。

· 更新:

标准简介

OVERVIEW

中文简介

该标准规定了水泥中氯化物、二氧化碳和碱含量的化学分析方法。它属于水泥试验方法系列标准的一部分,旨在为水泥的化学分析提供标准化的测试程序,包括试剂准备、仪器要求及具体操作步骤。

English summary

This standard specifies the chemical analysis methods for determining the chloride, carbon dioxide, and alkali content of cement. It is part of the series of standards on methods of testing cement, providing standardized test procedures including reagent preparation, apparatus requirements, and specific operational steps for chemical analysis.

以上为根据文件整理的内容简介。

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DIN EN 196PDF 第 1 页 · 原页码 1

4.2.8 Ammonium iron (III) sulphate, FeNH4(SO4)2 · 12H2O.

4.2.9 Indicator solution

Add 10 ml of dilute nitric acid (1 + 2) to 100 ml of a cold saturated solution of ammonium iron (III) sulfate in water.

4.3 Apparatus

4.3.1 Balance, capable of weighing to an accuracy of 0,0001 g.

4.3.2 10 ml burette, with 0,1 ml scale intervals.

4.3.3 Desiccator, containing anhydrous magnesium perchlorate, Mg(ClO4)2.

4.3.4 Filter paper, coarse (of about 20 μm pore diameter).

4.3.5 5 ml pipette.

4.4 Procedure

Weigh (5 ± 0,05) g of cement and place it in a 250 ml beaker, add 50 ml of water and, while stirring with a glass rod, 50 ml of dilute nitric acid (1 + 2) (4.2.2). Heat the mixture to boiling, stirring occasionally, and boil for one minute. Add, by pipetting (4.3.5), 5 ml of silver nitrate solution (4.2.5) to the boiling solution. Then boil for a maximum of one minute and filter through a filter paper (4.3.4) washed before use with dilute nitric acid (1 + 100) (4.2.3), into a 500 ml flask. Wash the beaker, glass rod and filter paper with dilute nitric acid (1 + 100) until the volume of the filtrate and washings is 200 ml. Cool the filtrate and washings to below 25 °C. Add 5 ml indicator solution (4.2.9) and titrate with the ammonium thiocyanate solution (4.2.7), shaking vigorously until a drop of this solution produces a faint reddish-brown colour which does not disappear on shaking. Record the volume, V1.

If the chloride content of cement exceeds 0,17 %, it will be necessary to repeat the test with a smaller quantity of cement.

Carry out the same procedure without cement sample (blank titration) and record the volume, V2, of ammonium thiocyanate solution used.

4.5 Expression of results

Calculate the chloride ions content, as a percentage, from the formula:

Cl− = (1,773 / 1000) · (V2 − V1) · (100 / m1) = 0,17733 · ((V2 − V1) / m1) (1)

where

m1 is the mass of cement test portion;

V1 is the volume of ammonium thiocyanate solution used for the titration of test solution;

V2 is the volume of ammonium thiocyanate solution used for the titration of blank solution.

Calculate the mean from the two results, to the nearest 0,01 %.

4.6 Repeatability and reproducibility

The repeatability standard deviation is 0,005 % and the reproducibility standard deviation 0,010 %.

5 Determination of carbon dioxide content (reference method)

5.1 Principle

The cement sample is treated with phosphoric acid to decompose the carbonate present. The carbon dioxide liberated is entrained in a current of carbon dioxide-free gas or air through a series of absorption tubes. The first two remove hydrogen sulfide and water and the following then absorb carbon dioxide. Two absorption tubes, each containing a granular absorbent for carbon dioxide and anhydrous magnesium perchlorate to retain the water formed during the absorption reaction are weighed to determine the mass of carbon dioxide released.

5.2 Reagents

5.2.1 Copper sulfate, CuSO4 · 5 H2O.

5.2.2 Copper sulfate solution, saturated.

5.2.3 Absorbent for hydrogen sulfide

Place a weighed quantity of dried pumice stone with a particle size between 1,2 mm and 2,4 mm into a flat dish and cover with a volume of saturated copper sulfate solution so that the mass of copper sulfate solution is approximately half that of the pumice stone. Evaporate the mixture to dryness, while stirring frequently with a glass rod. Dry the contents of the dish for at least five hours in an oven at a temperature of (155 ± 5) °C. Allow the solid mixture to cool in a desiccator and store in an airtight bottle.

5.2.4 Absorbent for water, anhydrous magnesium perchlorate, Mg(ClO4)2, with a particle size between 0,6 mm and 1,2 mm.

5.2.5 Absorbent for carbon dioxide, synthetic silicates with a particle size between 0,6 mm to 1,2 mm2), impregnated with sodium hydroxide, NaOH.

5.2.6 Concentrated phosphoric acid, H3PO4.

5.2.7 Concentrated sulfuric acid, H2SO4.

5.3 Apparatus

5.3.1 Apparatus for determining the carbon dioxide content

Figure 1 shows a typical apparatus which can be fitted with either a cylindrical pressure vessel, a small electrical compressor or a suitable suction pump which will ensure an even flow of gas or air.

The gas (air or nitrogen) entering the apparatus has previously had its carbon dioxide removed by first being passed through an absorbent (5.2.5). The apparatus consists of a 100 ml reaction flask (A) fitted with a three-neck adaptor, neck B1, being connected to a dropping funnel (O), neck B2 to a connecting tube and neck C to a water-cooled condenser. The funnel on B1 and the connecting tube on B2 are joined by means of a Y-piece (P), so that the carbon dioxide-free air can flow either through the connecting tube or the funnel, which can be controlled by means of a Mohr clip (N). After the condenser (L), the gas is passed through concentrated sulfuric acid (D), through absorption tubes containing the absorbent for hydrogen sulfide (5.2.3) (E) and

2) The absorbent is available ready for use.

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