GB/T 12960-2019 English PDF (GBT12960-2019)

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GB/T 12960-2019: Quantitative Determination of Constituents of Cement
GB/T 12960-2019
Quantitative determination of constituents of cement
ICS 91.100.10
Q11
National Standards of People's Republic of China
Replace GB/T 12960-2007
Quantitative determination of cement components
2019-10-18 released
2020-09-01 Implementation
State Administration for Market Regulation
Issued by China National Standardization Administration
Table of contents
Foreword Ⅰ
1 Scope 1
2 Normative references 1
3 Basic requirements of the test 1
4 Reagents and materials 2
5 Apparatus and equipment 3
6 Preparation of samples 4
7 Method for determination of cement components 5
8 Determination of cement components 2 8
9 Precision 10
Preface
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 12960-2007 "Quantitative Determination of Cement Components". Compared with GB/T 12960-2007, the main changes are as follows.
---In the scope, "applicable to general-purpose Portland cement (Portland cement, ordinary Portland cement, slag Portland cement, pozzolanic silica
The "determination of salt cement, fly ash Portland cement and composite Portland cement)" is revised to "applicable to granulated blast furnace
Pozzolanic mixed materials, fly ash, limestone, sandstone, kiln dust, gypsum, Portland cement clinker one or more of the water
Mud" (see Chapter 1, Chapter 1 of the.2007 edition).
---In the preparation of the sample, the "Sampling method of other mixed materials and other samples" is deleted, and only the cement sample is required (see Chapter 7 of the.2007 edition).
---Modified the relevant measurement conditions of the selective dissolution method.
● Use acid solution to select dissolving conditions, "control temperature at 10℃±2℃" amended to "control temperature at 20℃±2℃"; "Add
Add 40mL of hydrochloric acid (1 2) that has been kept in the water at 10℃±2℃ for 8min~10min (1 2)" is modified to "Add 50mL
Nitric acid (15) that has been heated in water at 20℃±2℃" (see 7.2.1, 8.2.1 of the.2007 edition);
● Select dissolution conditions for EDTA solution, "take 50mLEDTA solution, 10mL triethanolamine (1 2), 80mL water" to modify
Changed to "take 50mLEDTA solution, 10mL triethanolamine (12), 120mL water" (see 7.2.2,.2007 edition 8.2.2).
---In the alkali asbestos absorption weighing method, the "repeat this operation, ventilate for another 10 minutes, take it off, keep the temperature constant, and weigh until each tube is connected
The difference between the two consecutive weighing results does not exceed 0.0010g, and the last weighing value shall prevail" and "If the second U-shaped tube
If the mass change of 12 continuously exceeds 0.0010g, the first U-shaped tube 11 should be replaced and the test should be restarted" (see 8.2.3.1 of the.2007 edition).
--- Added the sulfide determination method to determine the components of granulated blast furnace slag (see 8.2.1).
---Added the burning weighing method, infrared analysis method and automatic photoelectric titration method for the determination of carbon dioxide (see 8.2.2, 8.2.3 and 8.2.4).
--- Added X-ray diffraction analysis method to determine gypsum composition (see 8.2.5).
--- Deleted the "potassium hydroxide-ethanol titration volumetric method" for the determination of carbon dioxide (see 8.2.3.2 in the.2007 edition).
---Modified the calculation formulas of various mixed material components and gypsum components in the standard.
---Deleted the calculation formula for the composition of cement produced by the shaft kiln (see 8.3.5.1, 8.3.5.2, 9.2.4.1, 9.2.4.2,.2007 edition)
10.2.3, 11.2.5.1, 11.2.5.2).
This standard was proposed by the China Building Materials Federation.
This standard is under the jurisdiction of the National Cement Standardization Technical Committee (SAC/TC184).
The main drafters of this standard. China Building Materials Inspection and Certification Group Co., Ltd., Shanghai Zhongcai Engineering Inspection Co., Ltd., Guangdong Province
Quality Supervision Cement Inspection Station (Meizhou), Southwest Anhui Product Quality Supervision and Inspection Center, China Building Materials Research Institute Co., Ltd., China
Cement Quality Supervision and Inspection Center, National Energy-saving Building Material Quality Supervision and Inspection Center (Hubei), Zhejiang Fangyuan Inspection Group Co., Ltd.
Company, Shandong Product Quality Inspection Research Institute, China Resources Cement Technology R and D Co., Ltd., Jiangsu Construction Engineering Building Material Quality Inspection Center Co., Ltd.,
China United Cement Group Co., Ltd., Zaozhuang China United Cement Co., Ltd., Hainan Product Quality Supervision and Inspection Institute, China Gezhouba Group Cement Co., Ltd.
The main drafters of this standard. Wang Ruihai, Zhang Qinghua, Wang Wei, Zhang Ge, Chen Rong, Lu Xiaoquan, Huang Dingce, Lu Juanjuan, Hong Runli, Liang Huichao,
Zhou Jianping, Liu Yamin, Wang Yalan, Tian Kun, Wang Qi, Dai Ping, Wu Heping, Wang Tao, Pang Yinghui, Zhang Ruiguo, Lin Yongquan, Ren Bingjian, Mei Guozheng, Zhu Zunfeng,
Liu Jinzhu, Huang Yan, Yang Lirong, Wang Guangdong, Cui Jian, Liu Miao.
The previous versions of the standard replaced by this standard are as follows.
---GB/T 12960-1991, GB/T 12960-1996, GB/T 12960-2007.
---GB/T 12961-1991.
Quantitative determination of cement components
1 Scope
This standard specifies Portland cement, ordinary Portland cement, slag Portland cement, pozzolanic Portland cement, fly ash silicate
Method for quantitative determination of cement and composite Portland cement components.
This standard applies to water containing granulated blast furnace slag, pozzolanic mixed materials, fly ash, limestone, sandstone, kiln dust, gypsum, and silicate
Cement of one or more materials in mud clinker.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 176 Cement chemical analysis method
GB/T 5484 Gypsum chemical analysis method
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
GB/T 12573 Cement sampling method
GB/T 35151 Method for determination of total organic carbon in limestone
3 Basic requirements of the test
3.1 Test times and requirements
The number of tests for each measurement is specified as two, and the average of the two test results is used to represent the measurement result.
The determination methods of cement components are divided into method one and method two. If multiple determination methods are listed for the same component, method one shall prevail when there is a dispute.
3.2 Laboratory temperature
The temperature of the laboratory is required to be between 16℃~30℃.
3.3 Constant
After the first drying or burning, cooling, and weighing, by continuously drying or burning the utensils or samples for 15 minutes each time, and then cooling,
The method of weighing to determine the constant mass, when the difference between two consecutive weighings is less than 0.0005g, the constant mass is reached.
3.4 Processing of results
3.4.1 Select the content of insoluble slag after dissolution, the content of carbon dioxide and the content of sulfur trioxide in terms of mass fraction, and the values are in percentage (%)
Expressed to two decimal places; the content of sulfide (calculated by S) is calculated by mass fraction, and the value is expressed as a percentage (%) to three decimal places.
3.4.2 The results of the determination of the content of each component in the cement are in mass fraction, and the value is expressed as a percentage (%) to one decimal place.
3.4.3 The rounding of values shall be carried out in accordance with GB/T 8170.
4 Reagents and materials
Unless otherwise stated, the reagents used should not be less than analytically pure. The water used should not be lower than the requirements of Grade 3 water specified in GB/T 6682.
Carbon dioxide-free water refers to water that is freshly boiled and cooled to room temperature.
4.1 Nitric acid (HNO3), density 1.39g/cm3~1.41g/cm3, mass fraction 65%~68%.
Note. The density of commercially available concentrated liquid reagents listed in this standard refers to the density (ρ) at 20°C, the same below.
4.2 Sulfuric acid (H2SO4), density 1.84g/cm3, mass fraction 95%~98%.
4.3 Phosphoric acid (H3PO4), density 1.68g/cm3, mass fraction ≥85%.
4.4 Triethanolamine [N(CH2CH2OH)3], density 1.12g/cm3, mass fraction 99%.
4.5 Ethanol (C2H5OH), the volume fraction is 95%.
4.6 Nitric acid (1 5).
Note 1.Use volume ratio to indicate the degree of reagent dilution, the same below. Nitric acid (15) means that 1 part by volume of concentrated nitric acid is mixed with 5 parts by volume of water.
Note 2.In chemical analysis, the acid used, where the concentration is not indicated, refers to the concentrated acid on the market.
4.7 Triethanolamine (1 2).
4.8 Sodium hydroxide solution (50g/L). Dissolve 5g sodium hydroxide (NaOH) in water, dilute to 100mL, and store in a plastic reagent bottle.
4.9 EDTA solution [c(EDTA)=0.15mol/L, c(NaOH)=0.25mol/L]. Weigh 55.8g disodium ethylenediaminetetraacetate
(C10H14N2O8Na2·2H2O) and 10g sodium hydroxide (NaOH), placed in a 1000mL beaker, add 500mL~600mL
Water, heat and stir to dissolve, filter, cool to room temperature and dilute with water to 1000mL, shake well.
4.10 Phosphate pH standard buffer solution. Weigh 2.238g disodium hydrogen phosphate (Na2HPO4 12H2O) and 0.851g potassium dihydrogen phosphate
(KH2PO4), accurate to 0.0001g, placed in a.200mL beaker, add about 100mL carbon dioxide-free water, warm and stir to make
Dissolve, cool to room temperature, transfer to a 250mL volumetric flask, wash the beaker with carbon dioxide-free water and dilute to the mark, shake.
The pH values of the phosphate pH standard buffer solutions at different temperatures are shown in Table 1.
4.11 Borate pH standard buffer solution. Weigh 0.953g sodium tetraborate (Na2B4O7·10H2O), accurate to 0.0001g, and place it in
In a.200mL beaker, add about 100mL carbon dioxide-free water, warm and stir to dissolve it, after cooling to room temperature, transfer to 250mL volume
In the measuring flask, wash the beaker with carbon dioxide-free water and dilute to the mark, and shake it well. The pH values of borate pH standard buffer solutions at different temperatures are shown in Table 1.
4.12 Copper sulfate (CuSO4·5H2O) saturated solution.
4.13 Hydrogen sulfide absorbent. Place the weighed dry pumice with a particle size of 1mm~2.5mm in a flat plate, and then use a fixed body
Soaked in saturated copper sulfate solution (see 4.12), the quality of the copper sulfate solution is about half of the mass of pumice. Put the mixture at 150℃±
In the drying oven (5.2) at 5°C, under constant stirring of the glass rod, evaporate the mixture to dryness, dry it for more than 5 hours, cool the solid mixture, and store it in a sealed bottle.
4.14 Soda lime, particle size 2mm~5mm, medical or chemically pure, sealed and stored.
4.15 Alkali asbestos, particle size 1mm~2mm (10 mesh ~ 20 mesh), chemically pure, sealed and stored.
4.16 Anhydrous magnesium perchlorate [Mg(ClO4)2], made into a particle size of 0.6mm~2mm, stored in a sealed bottle.
5 Apparatus and equipment
5.1 Balance, the graduation value is not more than 0.0001g.
5.2 Drying box, the temperature can be controlled at 105℃±5℃, 150℃±5℃.
5.3 Acidity meter, measuring pH value range 0~14, accurate to 0.02.
5.4 Glass sand core funnel, diameter 35mm~60mm, model G4 (average pore diameter 3μm~4μm).
The same specification glass sand core crucible can also be used.
5.5 Suction filter flask, 1000mL.
5.6 Air pump, pumping speed 0.25L/s.
5.7 Cement component measuring device, which can keep constant temperature of 20℃±2℃, as shown in Figure 1.
5.8 Carbon dioxide measuring device (alkali asbestos absorption weighing method), as shown in Figure 2.
Install a suitable suction pump and a glass rotor flow meter to ensure that the gas flows evenly through the device.
5.10 The high temperature furnace can control the temperature of 580℃±20℃, 950℃±25℃.
5.11 Dryer with color-changing silica gel inside.
5.12 Porcelain crucible with lid, capacity 20mL~30mL.
6 Preparation of samples
Cement samples are sampled according to the GB/T 12573 method, and the samples sent to the laboratory should be representative uniform samples. Quarters
Or the shrinkage divider will reduce the sample to about 100g, after sieving through a 150μm square-hole sieve, the residue on the sieve is grinded to make it all pass through
150μm square hole sieve, mix well, put it into a clean and dry sample bottle, and seal it.
Note. Prepare the sample as quickly as possible to prevent moisture absorption.
7 Cement component determination method 1
7.1 Principle
Pozzolanic mixed materials or fly ash components adopt selective dissolution method, cement samples are selectively dissolved with nitric acid solution, and pozzolanic mixed materials
Material or fly ash components are basically insoluble, while other components are basically dissolved.
The granulated blast furnace slag component adopts the selective dissolution method. After the cement sample is selectively dissolved by the pH 11.60 solution containing EDTA, the clinker,
Gypsum and carbonate are basically dissolved, while other components are basically insoluble.
The content of limestone is determined by the content of carbon dioxide. The determination of carbon dioxide adopts the alkali asbestos absorption weighing method.
From the results of selective dissolution and the content of carbon dioxide and sulfate sulfur trioxide in the cement, the content of each component in the cement is calculated.
Kiln ash is counted in pozzolanic mixed materials or fly ash components and limestone components.
Sandstone is counted in the pozzolanic mixture or fly ash component.
7.2 Test procedure
7.2.1 Determination of insoluble residue content after selective dissolution with nitric acid solution
Weigh 0.5000g±0.0200g sample (m3), accurate to 0.0001g, place it in a.200mL dry beaker, add 80mL water,
Put in a stir...