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GB/T 176-2017 (GBT176-2017)

GB/T 176-2017_English: PDF (GBT 176-2017, GBT176-2017)
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BASIC DATA
Standard ID GB/T 176-2017 (GB/T176-2017)
Description (Translated English) Methods for chemical analysis of cement
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard Q11
Classification of International Standard 91.100.10
Word Count Estimation 78,730
Date of Issue 2017-12-29
Date of Implementation 2018-11-01
Drafting Organization China Building Materials Inspection & Certification Group Co., Ltd., Shanghai Zhongcai Engineering Inspection Co., Ltd., China Building Materials Inspection & Certification Group Jiangsu Co., Ltd., Guangdong Quality Supervision Cement Inspection Station (Guangzhou), Tianjin Jinbei Construction Engineering Test & Inspection Technology Co., Ltd., China Construction Materials Science Research Institute
Administrative Organization National Cement Standardization Technical Committee (SAC/TC 184)
Proposing organization China Federation of Building Materials
Issuing agency(ies) General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, China National Standardization Administration

Standards related to: GB/T 176-2017

GB/T 176-2017
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 91.100.10
Q 11
Replacing GB/T 176-2008
Methods for chemical analysis of cement
(ISO 29581-1:2009 Cement - Test methods -
Part 1: Analysis by wet chemistry, NEQ)
ISSUED ON: DECEMBER 29, 2017
IMPLEMENTED ON: NOVEMBER 01, 2018
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 6 
1 Scope ... 11 
2 Normative references ... 11 
3 Terms and definitions ... 12 
4 Basic requirements for test ... 13 
4.1 Number of tests and requirements ... 13 
4.2 Representation of mass, volume, titer and results ... 13 
4.3 Repeatability limit and reproducibility limit ... 13 
4.4 Blank test ... 14 
4.5 Burning ... 14 
4.6 Constant mass ... 14 
4.7 Checking chloride (silver nitrate inspection) ... 14 
4.8 General requirements for reagents ... 15 
4.9 Verification of test methods ... 15 
5 Preparation of specimens ... 15 
6 Chemical analysis methods ... 16 
6.1 Reagents and materials ... 16 
6.2 Instruments and equipment ... 42 
6.3 Determination of loss on ignition of cement - Ignition difference method ... 47 
6.4 Determination of loss on ignition of slag Portland cement - Correction method
(reference method) ... 48 
6.5 Determination of sulfate sulfur trioxide - Barium sulfate gravimetric method
(reference method) ... 50 
6.6 Determination of insoluble matter - Hydrochloric acid-sodium hydroxide
treatment ... 51 
6.7 Determination of silica - Ammonium chloride gravimetric method (reference
method) ... 53 
6.8 Determination of ferric oxide - Phenanthroline spectrophotometric method
(reference method) ... 56 
6.9 Determination of aluminum oxide - EDTA direct titration of iron and aluminum
content (reference method) ... 57 
6.10 Determination of calcium oxide - EDTA titration method (reference method)
... 58 
6.11 Determination of magnesium oxide - Atomic absorption spectrophotometry
(reference method) ... 59 
6.12 Determination of titanium dioxide - Diantipyrine methane spectrophotometry
... 61 
6.13 Determination of chloride ion - Ammonium thiocyanate volumetric method
(reference method) ... 62 
6.14 Determination of potassium oxide and sodium oxide - Flame photometry
(reference method) ... 63 
6.16 Determination of manganese monoxide - Potassium periodate oxidation
spectrophotometry (reference method) ... 66 
6.17 Determination of phosphorus pentoxide - Phosphorus molybdenum blue
spectrophotometric method ... 67 
6.18 Determination of carbon dioxide - Soda asbestos absorption gravimetric
method ... 69 
6.19 Determination of zinc oxide - Atomic absorption spectrophotometry ... 70 
6.20 Determination of silicon dioxide - Potassium fluorosilicate volumetric method
... 71 
6.21 Determination of ferric trioxide - EDTA direct titration method (alternative
method) ... 73 
6.22 Determination of ferric trioxide - Atomic absorption spectrophotometry
(alternative method) ... 74 
6.23 Determination of aluminum oxide - EDTA direct titration method (alternative
method) ... 75 
6.24 Determination of aluminum oxide - Copper sulfate back titration method ... 76 
6.25 Determination of calcium oxide - Melted sodium hydroxide-EDTA titration
method (alternative method) ... 77 
6.26 Determination of calcium oxide - Potassium permanganate titration
(alternative method) ... 78 
6.27 Determination of magnesium oxide - EDTA titration subtraction method
(alternative method) ... 80 
6.28 Determination of sulfur trioxide sulfate - Iodometric method ... 82 
6.29 Determination of sulfur trioxide sulfate - Coulometric titration ... 85 
6.30 Determination of sulfur trioxide sulfate - Ion exchange method (alternative
method) ... 86 
6.31 Determination of chloride ions - (Automatic) potentiometric titration method
(alternative method) ... 87 
6.32 Determination of chloride ions - Ion chromatography (alternative method) . 89 
6.33 Determination of potassium oxide and sodium oxide - Atomic absorption
spectrophotometry (alternative method) ... 90 
6.34 Determination of manganese monoxide - Atomic absorption
spectrophotometry (alternative method) ... 91 
6.35 Determination of fluoride ion - Ion selective electrode method ... 92 
6.36 Determination of free calcium oxide - Glycerol method (alternative method)
... 93 
6.37 Determination of free calcium oxide - Glycol method (alternative method) . 94 
6.38 Determination of free calcium oxide - Ethylene glycol extraction-EDTA titration
(alternative method) ... 95 
6.39 Determination of loss on ignition of slag Portland cement - Correction method
(alternative method) ... 96 
6.40 Determination of total sulfur in Portland cement raw material ... 98 
6.41 Limits of repeatability and reproducibility of the results of chemical analysis
methods of cement ... 98 
7 X-ray fluorescence analytical methods ... 100 
7.1 Method summary ... 100 
7.2 Reagents ... 100 
7.3 Instruments and equipment ... 103 
7.4 Preparation of test pieces ... 104 
7.5 Calibration and verification ... 107 
7.6 Calculation and representation of results ... 115 
7.7 Repeatability and reproducibility limits of determination results by X-ray
fluorescence analysis method ... 115 
8 Inductively coupled plasma emission spectroscopy ... 116 
8.1 Method summary ... 116 
8.2 Reagents ... 116 
8.3 Instruments and equipment ... 121 
8.4 Determination of ferric oxide, aluminum oxide, magnesium oxide, titanium
oxide, potassium oxide, sodium oxide, manganese oxide, zinc oxide, phosphorus
pentoxide ... 121 
8.5 Determination of sulfur trioxide sulfate ... 122 
8.6 Repeatability and reproducibility limits of the determination results by ICP-AES
... 123 
Appendix A (Informative) Example for calculation of metering point in
potentiometric titration for chloride ion ... 124 
Appendix B (Informative) Reference chromatographic conditions and
chromatograms of carbonate eluent ... 125 
Appendix C (Informative) Recommended wavelength for inductively coupled
plasma emission spectroscopy ... 126 
Foreword
This standard is drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 176-2008 "Methods for chemical analysis of
cement". Compared with GB/T 176-2008, the main changes are as follows:
- In the Scope, ADD the inductively coupled plasma emission spectroscopy
(see Chapter 1; Chapter 1 of the 2008 edition).
- MODIFY that "During chemical analysis, unless otherwise specified, it shall
carry out the determination of loss on ignition simultaneously" into "During
chemical analysis, it is recommended to determine loss on ignition
simultaneously" (see 4.1; 4.1 of the 2008 edition).
- ADD that "Unless otherwise stated, the validity period of the standard
titration solution is 3 months; if it exceeds 3 months, it shall be calibrated
again" (see 4.8).
- For the preparation of the specimen, MODIFY that "all passes through a
square hole sieve which has an aperture of 80 μm" into "all passes through
a square hole sieve which has an aperture of 150 μm". MODIFY that "The
use of magnets to remove metallic iron from the sieve residue" into "if the
metallic iron carried in the sample preparation process may affect the
determination of related chemical properties, use the magnet to remove
metallic iron from the sieve residue". In the prompt, ADD that "Before
analyzing cement and cement clinker specimen, it does not require drying
the specimen" (see Chapter 5; Chapter 7 of the 2008 edition).
- For the calibration of sodium thiosulfate standard titration solution,
CHANGE from "potassium dichromate standard titration solution" to
"potassium iodate standard titration solution" (see 6.1.85.2; 5.84.2 of the
2008 edition).
- The determination of loss on ignition is divided into "determination of loss
on ignition of cement" and "determination of loss on ignition of slag Portland
cement". In the determination of the loss on ignition of slag Portland cement,
MAKE specific requirements for the determination method of sulfate sulfur
trioxide in the sample material (see 6.3, 6.4, 6.39; Chapter 8 of the 2008
edition).
- MODIFY the "sulfur trioxide" into "sulfate sulfur trioxide" (see 6.5, 6.28, 6.29,
6.30; Chapter 10, Chapter 30, Chapter 31, Chapter 33 of 2008 edition).
- Determination of sulfate sulfur trioxide - In the barium sulfate gravimetric
method (reference method), MODIFY the decomposition time of the
(see 6.19).
- Determination of silicon dioxide - In the potassium fluorosilicate volumetric
method (alternative method), MODIFY that "Add 10 mL ~ 15 mL of nitric
acid" into "Add 15 mL of nitric acid"; MODIFY that "place it under 30 °C for
15 min ~ 20 min" into "place it at 10 °C ~ 26 °C for 15 min ~ 20 min" (See
6.20; Chapter 23 of the 2008 edition).
- Determination of ferric oxide - In the EDTA direct titration method
(alternative method), MODIFY "pH 1.8 ~ 2.0" into "pH 1.8" (See 6.21;
Chapter 12 of the 2008 edition).
- Determination of aluminum trioxide - In the copper sulfate back titration
method (alternative method), ADD that if the consumption of the copper
sulfate standard titration solution is less than 10 mL, increase the amount
of EDTA standard titration solution and retest (See 6.24; Chapter 26 of the
2008 edition).
- Determination of sulfate sulfur trioxide - In the coulometric titration method
(alternative method), MODIFY that "When there is sulfur in other states
besides sulfide (S2-) and sulfate in the specimen, it will cause an error in
the determination result." into “When the sample contains a large amount
of sulfide (S2-) or sulfur in other states, the sulfur or other state of sulfur may
not be completely decomposed by formic acid, which will cause a positive
error in the determination result, such as the cement which is mixed of a
large amount of slag” (see 6.29; Chapter 33 of the 2008 edition).
- Determination of sulfate sulfur trioxide - In the ion-exchange method
(alternative method), ADD the requirements that "this method is only used
for enterprise production control" (see 6.30; Chapter 31 of the 2008 edition).
- DELETE the determination of sulfur trioxide - Barium chromate
spectrophotometry (alternative method) (Chapter 32 of the 2008 edition).
- ADD the determination of chloride ion - (Automatic) potentiometric titration
method (alternative method) (see 6.31).
- ADD the determination of chloride ions - Ion chromatography (alternative
method) (see 6.32).
- DELETE the determination of chloride ion - Phosphoric acid distillation-
Mercury salt titration method (alternative method) (Chapter 35 of the 2008
edition).
- In the determination of free calcium oxide - In the ethylene glycol method
(alternative method), DELETE that “extraction filtration 4 min after heating
to slight boiling” in the analytical procedures; MODIFY it into “titration
Environment and Green Building Experiment Center Co., Ltd., Qinghai Institute
of Building Materials Science, Guangdong Building Research Institute Group
Co., Ltd., Bayingoleng Mongolian Autonomous Prefecture Product Quality
Inspection Institute, Jiangsu Construction Engineering Quality Inspection
Center Co., Ltd., Boai Jinyu Cement Co., Ltd., Huarun Cement R&D Center,
Yunnan Building Material Product Quality Supervision and Inspection Station,
Shandong Province Cement Quality Supervision and Inspection Station,
Shandong Province Product Quality Inspection Research Institute, Beijing Jinyu
Cement Energy-saving Technology Co., Ltd., Inner Mongolia Autonomous
Region Building Material Product Quality Inspection Institute, Tianjin
Construction Material Product Quality Supervision and Inspection Center,
Heilongjiang Construction Material Quality Supervision and Inspection Station,
Hainan Province Product Quality Supervision and Inspection Institute, Beijing
Construction Engineering Quality First Inspection Institute Co., Ltd.,
Guangdong Shaoguan Quality Metrology Supervision and Inspection Institute,
Guangdong Qingyuan Quality Metrology Supervision and Inspection Institute,
Sichuan Esheng Cement Group Co., Ltd., China Gezhouba Group Cement Co.,
Ltd., Shimadzu Enterprise Management (China) Co., Ltd., China United
Cement Group Co., Ltd., Zaozhuang Zhonglian Cement Co., Ltd., Zibo Luzhong
Cement Co., Ltd., Tai Ni (Guigang) Cement Co., Ltd., Hebei Jinyu Dingxin
Cement Co., Ltd., Liqiang Technology (Shanghai) Co., Ltd.
The main drafters of this standard: Wang Ruihai, Zhang Qinghua, Cui Jinhua,
Cui Jian, Yang Weiping, Zhu Xiaohong, Wang Wei, Liang Huichao, Yu Ligang,
Wang Xinli, Yu Kexiao, Dai Ping, Lu Juanjuan, Liu Yubing, Qu Xueying, Shen
Hongmei, Deng Wenhong, Wang Hong, Wu Heping, Deng Lijuan, Liu Chunmei,
Zhang Feifei, Wang Yuanguang, Ma Lijun, Zhang Yating, Zhang Yongsheng,
Lin Yongquan, Ren Bingjian, Zhou Guilin, Li Feng, Zou Xin, Dong Xiaoli, Zhai
Lijuan, Fang Yue, Wu Zhiwei, Huang Yan, Cheng Yunyun, Tang Shanshan Xue
Xue, Zeng Weijun, Deng Lei, Fu Xiaohong, Song Xiaohong, Li Liangfeng, Li
Baoming, Wang Huiqiang, Gao Yuansheng, Wu Zhenping, Li Zhibo, Wang
Yalan, Wang Qi, Liu Yamin, Guo Meng, Zhang Ge.
This standard replaces the standard previously issued as follows:
- GB/T 176-1956, GB/T 176-1962, GB/T 176-1976, GB/T 176-1987, GB/T
176-1996, GB/T 176-2008;
- GB/T 19140-2003.
Methods for chemical analysis of cement
1 Scope
This standard specifies methods for chemical analysis of cement, X-ray
fluorescence analysis methods, inductively coupled plasma emission
spectrometry for the determination of loss on ignition (LOI), SO3, insoluble (IR),
SiO2, Fe2O3, Al2O3, CaO, MgO, TiO2, Cl-, K2O, Na2O, S2-, MnO, P2O5, CO2, ZnO,
F-, free calcium oxide (fCaO), SrO. Chemical analysis methods of cement are
further divided into reference methods and alternative methods. If multiple
determination methods are listed for the same component, the reference
method shall prevail in case of dispute.
This standard applies to general Portland cement, clinker, raw material for the
preparation of the above cement, other cements and materials designated to
use this standard.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 5762 Methods for chemical analysis of limestone, quicklime and
hydrated lime for building materials industry
GB/T 6682 Water for analytical laboratory use - Specifications and test
methods
GB/T 8170 Rules for rounding off for numerical values & expression and
judgement of limiting values
GB/T 12573 Sampling method for cement
GB/T 15000 (all parts) Directives for the work of reference materials
GSB 08-1110 Standard sample of cement raw materials for X-ray
fluorescence analysis
GSB 08-1355 Standard sample for analysis of cement clinker composition
GSB 08-1356 Standard sample for composition analysis of ordinary Portland
A set of standard samples used for calibrating analytical instruments such
as X-ray fluorescence analyzer which is related to chemical composition.
4 Basic requirements for test
4.1 Number of tests and requirements
The number of tests for each determination is specified as two; the absolute
difference between the two results is within the repeatability limit (Table 3, Table
4, Table 5). The average value of the two test results is used to indicate the
determination result.
During routine production control analysis, the number of tests for each
determination may be one.
In chemical analysis, it is recommended to determine the loss on ignition at the
same time.
Except for the loss on ignition, it shall perform other blank tests simultaneously
and correct the determination results.
4.2 Representation of mass, volume, titer and results
Mass is expressed in "grams (g)" and is accurate to 0.0001 g. The volume of
the burette is expressed in "milliliter (mL)"; the reading is accurate to 0.01 mL.
The titer is expressed in "milligrams per milliliter (mg/mL)".
The titer of benzoic acid-anhydrous ethanol standard titration solution for the
titer of calcium oxide retains three significant figures; the concentration, titer
and volume ratio of other standard titration solutions retain four significant
figures.
Unless otherwise stated, all analysis results are based on mass fraction. The
results of chloride ion analysis are expressed as % to three digits after the
decimal point; the other analysis results are expressed as % to two digits after
the decimal point.
The rounding of the value is performed according to GB/T 8170.
4.3 Repeatability limit and reproducibility limit
The repeatability limits and reproducibility limits listed in this standard are
absolute deviations, expressed in terms of mass fraction (%).
by the use of silver nitrate.
4.8 General requirements for reagents
Unless otherwise specified, the reagents used shall not be lower than analytical
grade; the reagents used for calibration shall be reference reagents. The water
used shall not be lower than the requirements of the third-grade water as
specified in GB/T 6682.
The density of the commercially available concentrated liquid reagents listed in
this standard refers to the density (ρ) at 20 °C, in the unit of grams per cubic
centimeter (g/cm3).
In chemical analysis, the acid or ammonia used, where no concentration is
indicated, refers to commercially available concentrated acid or ammonia.
Use the volume ratio to indicate the degree of dilution of the reagent, for
example: hydrochloric acid (1 + 2) means that 1 part of concentrated
hydrochloric acid is mixed with 2 parts of water.
Unless otherwise stated, the validity period of the standard titration solution is
3 months. If it exceeds 3 months, recalibrate it.
4.9 Verification of test methods
The test methods listed in this standard can be compared with certified standard
samples / standard materials (such as GSB 08-1110, GSB 08-1355, GSB 08-
1356, GSB 08-1357, GSB 08-2985) to verify the accuracy of the method.
5 Preparation of specimens
Take sample according to the method of GB/T 12573. The sample sent to the
laboratory shall be a representative uniform sample. The sample is divided to
about 100 g by a quartering method or a divider. After sieving through a 150 μm
square hole sieve, the debris is removed. After the sieve residue is ground, it is
passed through a 150 μm square hole sieve. Make it thoroughly mixed and
contained into a clean, dry sample bottle. Seal it. Mix it further to prepare for
the use of determination.
If the metallic iron carried in the sample preparation process may affect the
determination of related chemical properties, use a magnet to remove the
metallic iron from the sieve residue.
Tip: Prepare the specimen as quickly as possible to prevent moisture
...