1 Scope
This standard specifies methods for chemical analysis and X-ray fluorescence analysis of cement. The methods for chemical analysis of cement are divided into reference method and substitution method. In case of disagreement, method for chemical analysis of cement shall be subject to reference method.
This standard is applicable to common portland cement and clinker and raw meal for preparing cements above, as well as other cement and materials that this Standard apply.
2 Normative References
The following standards contain provisions which, through reference in this text, constitute provisions of this standard.For dated reference, subsequent amendments (excluding amending error in the text) to, or revisions of, any of these publications do not be applied. However, the parties whose enter into agreement according to these specifications are encouraged to research whether the latest editions of these references are applied or not. For undated references, the latest edition of the normative document is applicable to these specifications.
GB/T 6682 Water for analytical laboratory use -- Specification and test methods (GB/T 6682-2008, ISO 3696: 1987, MOD)
GB/T 12573 Sampling Method for Cement
GB/T 15000 Directives for the work of reference materials (All the parts)
GBW 03201 Composition analysis of portland cement -- standard sample
GBW 03204 Composition analysis of cement clinker -- standard sample
GBW 03205 Composition analysis of ordinary portland cement -- standard sample
GSB 08-1355 composition analysis of cement clinker -- standard sample
GSB 08-1356 Composition analysis of ordinary portland cement -- standard sample
GSB 08-1357 Composition analysis of portland cement -- standard sample
JC/T 1085 X-ray fluorescence analyzer for cement
JJG 1006 Technical Norm of Primary Reference Material
3 Terms and Definitions
For the purpose of this standard, the terms and definitions established in GB/T 15000 (All the parts) as well as the following ones apply.
3.1
Repeatability conditions
Conditions where the measured objects are tested with the same method on identical test items (material) in the same laboratory by the same operator using the same equipment within short intervals of time.
3.2
Reproducibility conditions
Conditions where the measured objects are tested with the same method on identical test items (material) in different laboratories with different operators using different equipment.
3.3
Repeatability limit
A value, under the repeatability conditions (3.1), that the absolute difference of two test resulta is less than or equal to this value in a probability of 95%.
3.4
Reproducibility limit
A value, under the reproducibility conditions (3.2), that the absolute difference of two test resulta is less than or equal to this value in a probability of 95%.
3.5
Calibration materials
A batch of material used for calibration of analytical instrument, which enables the physical quantity gained by the analytical instrument correlate with the corresponding mass fraction of chemical composition.
3.6
Certified reference materials for X-ray fluorescence analysis
Complete set of certified reference materials that are used tocalibrate the correlation of analytical instruments like X-ray fluorescence analyzer to chemical composition.
3.7
Beads
Material pieces for analyzing surface smoothness and detecting defects like apparent crack, which are made by placing the material melten by fluxing agent in a special mould and cooling them under the specific cooling conditions.
3.8
Anti-wetting agents
Substance used to avoid cracking of fuse piece in beads cooling and to facilitate stripping.
3.9
Pellets
Material pieces with cetain strength, for analyzing surface smoothness and detecting defects like crack, which are made by making the material to powders wot a specific fineness and extrusion forming under the specific conditions.
3.10
Binding agent
Substance that enables the material be easy to form by high pressure free from measured elements or special absorption / enhancement effect on the measured elements.
4 Basic Requirements of Test
4.1 Number and requirements and tests
The number of tests for each determination shall be two, and the mean value of two test results shall be adoptedas the determination result.
In routine production control analyzing, the number of tests for each determination may be one.
In chemical analysis, unless otherwise stated, ignition loss shall also be tested; in other determinations, blank test shall be carried in parall, and the test results shall be calibrated.
4.2 Expression of masses, volumes, titer values and results
Express masses in grams to the nearest 0.000 1 g; volumes from burettes in millilitres to the nearest 0.05 ml; and titer values in milligram per milliliter (mg/mL).
Epress the titer values of mercuric nitrate standard volumetric solution to chloride ion, after rouding off, to three decimal places; the titer values and volume ratios of other standard volumetric solutions to four decimal places.
Unless otherwise stated, express the analysis results by mass fraction; and express the analysis result for chloride ion, as a percentage generally to three decimal places, and other analysis results as a percentage generally to two decimal places.
4.3 Blank determination
Carry out a blank determination without a sample, where relevant, following the same procedure and using the same amounts of reagents. Correct the results obtained for the determination accordingly.
4.4 Ignitions
Place the filter paper and its preciptiate contents into a crucible which has been previously ignited and tared. Dry it, then incinerate slowly in an oxidising atmosphere in order to avoid immediate flaming, while ensuring complete combustion. Place the crucible in a high temperature furnace (6.7) after incinerating the contents to the state without black carbon grains. Ignite the crucible and its contents at the stated temperature then allow to cool to the laboratory temperature in a desiccator (6.5). Weigh the crucible and its contents.
1 Scope
2 Normative References
3 Terms and Definitions
4 Basic Requirements of Test
5 Reagents and Materials
6 Apparatus
7 Preparation of a Test Sample of Cement
8 Determination of Loss on Ignition -Ignition Subtraction Method
9 Determination of Residue Insoluble - Hydrochloric Acid and Sodium Hydroxide
10 Determination of Sulfur Trioxide - Barium Sulfate Gravimetric Method (Reference Method)
11 Determination of Silica - Ammonium Chloride Gravimetric Method (Reference Method)
12 Determination of Ferric Oxide - EDTA Direct Titration (Reference Method)
13 Determination of Aluminum Oxide - EDTA Direct Titration (Reference Method)
14 Determination of Calcium Oxide - EDTA Titration (Reference Method)
15 Determination of Magnesium Oxide - Atomic Absorption Spectrometry (Reference Method)
16 Determination of Titanium Dioxide - Diantipyrylmethane Spectrophotometric Method
17 Determination of Potassium Oxide and Sodium Oxide - Flame Photometry (Reference Method)
18 Determination of Chloride - Ammonium Thiocyanate Volumetric Method (Reference Method)
19 Determination of Sulfide-Iodometry
20 Determination of Manganous Oxide-Potassium Periodate Oxidation Spectrophotometry (Reference Method)
21 Determination of Phosphorus Pentoxide-Ammonium Phosphomolybdate Spectrophotometry
22 Determination of Carbon Dioxide-Alkali Asbestos Absorption Gravimetric Method
23 Determination of Silicon Dioxide-Potassium Fluosilicate Volumetric Method (Alternative Method)
24 Determination of Ferric Oxide-Phenanthroline Spectrophotometry (Alternative Method)
25 Determination of Ferric Oxide-Atomic Absorption Spectrometry (Alternative Method)
26 Determination of Aluminium Oxide-Copper Sulfate Back Titration (Alternative Method)
27 Determination of Calcium Oxide-Sodium Hydroxide Fusion-EDTA Titration (Alternative Method)
28 Determination of Calcium Oxide-Potassium Permanganate Titration (Alternative Method)
29 Determination of Magnesium Oxide-EDTA Titration Subtraction Method (Alternative Method)
30 Determination of Sulfur Trioxide-Iodometry (Alternative Method)
31 Determination of Sulfur Trioxide-Ion Exchange Method (Alternative Method)
32 Determination of Sulfur Trioxide-Barium Chromate Spectrophotometry (Alternative Method)
33 Determination of Sulfur Trioxide-Coulometry (Alternative Method)
34 Determination of Potassium Oxide and Sodium Oxide-Atomic Absorption Spectrometry (Alternative Method)
35 Determination of Chloride Ion-Phosphoric Acid Distillation-Mercury Salts Titration (Alternative Method)
36 Determination of Manganous Oxide-Atomic Absorption Spectrometry (Alternative Method)
37 Determination of Fluorine Ion-Ion Selective Electrode Method
38 Determination of Free Calcium Oxide-Glycidol Method (Alternative Method)
39 Determination of Free Calcium Oxide-Ethylene Glycol Method (Alternative Method)
40 X-ray Fluorescence Analysis Method
41 Repeatability Limit and Reproducibility Limit of Determination Results with Methods for Chemical Analysis of Cement and X-ray Fluorescence Analysis Methods
1 Scope
This standard specifies methods for chemical analysis and X-ray fluorescence analysis of cement. The methods for chemical analysis of cement are divided into reference method and substitution method. In case of disagreement, method for chemical analysis of cement shall be subject to reference method.
This standard is applicable to common portland cement and clinker and raw meal for preparing cements above, as well as other cement and materials that this Standard apply.
2 Normative References
The following standards contain provisions which, through reference in this text, constitute provisions of this standard.For dated reference, subsequent amendments (excluding amending error in the text) to, or revisions of, any of these publications do not be applied. However, the parties whose enter into agreement according to these specifications are encouraged to research whether the latest editions of these references are applied or not. For undated references, the latest edition of the normative document is applicable to these specifications.
GB/T 6682 Water for analytical laboratory use -- Specification and test methods (GB/T 6682-2008, ISO 3696: 1987, MOD)
GB/T 12573 Sampling Method for Cement
GB/T 15000 Directives for the work of reference materials (All the parts)
GBW 03201 Composition analysis of portland cement -- standard sample
GBW 03204 Composition analysis of cement clinker -- standard sample
GBW 03205 Composition analysis of ordinary portland cement -- standard sample
GSB 08-1355 composition analysis of cement clinker -- standard sample
GSB 08-1356 Composition analysis of ordinary portland cement -- standard sample
GSB 08-1357 Composition analysis of portland cement -- standard sample
JC/T 1085 X-ray fluorescence analyzer for cement
JJG 1006 Technical Norm of Primary Reference Material
3 Terms and Definitions
For the purpose of this standard, the terms and definitions established in GB/T 15000 (All the parts) as well as the following ones apply.
3.1
Repeatability conditions
Conditions where the measured objects are tested with the same method on identical test items (material) in the same laboratory by the same operator using the same equipment within short intervals of time.
3.2
Reproducibility conditions
Conditions where the measured objects are tested with the same method on identical test items (material) in different laboratories with different operators using different equipment.
3.3
Repeatability limit
A value, under the repeatability conditions (3.1), that the absolute difference of two test resulta is less than or equal to this value in a probability of 95%.
3.4
Reproducibility limit
A value, under the reproducibility conditions (3.2), that the absolute difference of two test resulta is less than or equal to this value in a probability of 95%.
3.5
Calibration materials
A batch of material used for calibration of analytical instrument, which enables the physical quantity gained by the analytical instrument correlate with the corresponding mass fraction of chemical composition.
3.6
Certified reference materials for X-ray fluorescence analysis
Complete set of certified reference materials that are used tocalibrate the correlation of analytical instruments like X-ray fluorescence analyzer to chemical composition.
3.7
Beads
Material pieces for analyzing surface smoothness and detecting defects like apparent crack, which are made by placing the material melten by fluxing agent in a special mould and cooling them under the specific cooling conditions.
3.8
Anti-wetting agents
Substance used to avoid cracking of fuse piece in beads cooling and to facilitate stripping.
3.9
Pellets
Material pieces with cetain strength, for analyzing surface smoothness and detecting defects like crack, which are made by making the material to powders wot a specific fineness and extrusion forming under the specific conditions.
3.10
Binding agent
Substance that enables the material be easy to form by high pressure free from measured elements or special absorption / enhancement effect on the measured elements.
4 Basic Requirements of Test
4.1 Number and requirements and tests
The number of tests for each determination shall be two, and the mean value of two test results shall be adoptedas the determination result.
In routine production control analyzing, the number of tests for each determination may be one.
In chemical analysis, unless otherwise stated, ignition loss shall also be tested; in other determinations, blank test shall be carried in parall, and the test results shall be calibrated.
4.2 Expression of masses, volumes, titer values and results
Express masses in grams to the nearest 0.000 1 g; volumes from burettes in millilitres to the nearest 0.05 ml; and titer values in milligram per milliliter (mg/mL).
Epress the titer values of mercuric nitrate standard volumetric solution to chloride ion, after rouding off, to three decimal places; the titer values and volume ratios of other standard volumetric solutions to four decimal places.
Unless otherwise stated, express the analysis results by mass fraction; and express the analysis result for chloride ion, as a percentage generally to three decimal places, and other analysis results as a percentage generally to two decimal places.
4.3 Blank determination
Carry out a blank determination without a sample, where relevant, following the same procedure and using the same amounts of reagents. Correct the results obtained for the determination accordingly.
4.4 Ignitions
Place the filter paper and its preciptiate contents into a crucible which has been previously ignited and tared. Dry it, then incinerate slowly in an oxidising atmosphere in order to avoid immediate flaming, while ensuring complete combustion. Place the crucible in a high temperature furnace (6.7) after incinerating the contents to the state without black carbon grains. Ignite the crucible and its contents at the stated temperature then allow to cool to the laboratory temperature in a desiccator (6.5). Weigh the crucible and its contents.
Contents of GB/T 176-2008
1 Scope
2 Normative References
3 Terms and Definitions
4 Basic Requirements of Test
5 Reagents and Materials
6 Apparatus
7 Preparation of a Test Sample of Cement
8 Determination of Loss on Ignition -Ignition Subtraction Method
9 Determination of Residue Insoluble - Hydrochloric Acid and Sodium Hydroxide
10 Determination of Sulfur Trioxide - Barium Sulfate Gravimetric Method (Reference Method)
11 Determination of Silica - Ammonium Chloride Gravimetric Method (Reference Method)
12 Determination of Ferric Oxide - EDTA Direct Titration (Reference Method)
13 Determination of Aluminum Oxide - EDTA Direct Titration (Reference Method)
14 Determination of Calcium Oxide - EDTA Titration (Reference Method)
15 Determination of Magnesium Oxide - Atomic Absorption Spectrometry (Reference Method)
16 Determination of Titanium Dioxide - Diantipyrylmethane Spectrophotometric Method
17 Determination of Potassium Oxide and Sodium Oxide - Flame Photometry (Reference Method)
18 Determination of Chloride - Ammonium Thiocyanate Volumetric Method (Reference Method)
19 Determination of Sulfide-Iodometry
20 Determination of Manganous Oxide-Potassium Periodate Oxidation Spectrophotometry (Reference Method)
21 Determination of Phosphorus Pentoxide-Ammonium Phosphomolybdate Spectrophotometry
22 Determination of Carbon Dioxide-Alkali Asbestos Absorption Gravimetric Method
23 Determination of Silicon Dioxide-Potassium Fluosilicate Volumetric Method (Alternative Method)
24 Determination of Ferric Oxide-Phenanthroline Spectrophotometry (Alternative Method)
25 Determination of Ferric Oxide-Atomic Absorption Spectrometry (Alternative Method)
26 Determination of Aluminium Oxide-Copper Sulfate Back Titration (Alternative Method)
27 Determination of Calcium Oxide-Sodium Hydroxide Fusion-EDTA Titration (Alternative Method)
28 Determination of Calcium Oxide-Potassium Permanganate Titration (Alternative Method)
29 Determination of Magnesium Oxide-EDTA Titration Subtraction Method (Alternative Method)
30 Determination of Sulfur Trioxide-Iodometry (Alternative Method)
31 Determination of Sulfur Trioxide-Ion Exchange Method (Alternative Method)
32 Determination of Sulfur Trioxide-Barium Chromate Spectrophotometry (Alternative Method)
33 Determination of Sulfur Trioxide-Coulometry (Alternative Method)
34 Determination of Potassium Oxide and Sodium Oxide-Atomic Absorption Spectrometry (Alternative Method)
35 Determination of Chloride Ion-Phosphoric Acid Distillation-Mercury Salts Titration (Alternative Method)
36 Determination of Manganous Oxide-Atomic Absorption Spectrometry (Alternative Method)
37 Determination of Fluorine Ion-Ion Selective Electrode Method
38 Determination of Free Calcium Oxide-Glycidol Method (Alternative Method)
39 Determination of Free Calcium Oxide-Ethylene Glycol Method (Alternative Method)
40 X-ray Fluorescence Analysis Method
41 Repeatability Limit and Reproducibility Limit of Determination Results with Methods for Chemical Analysis of Cement and X-ray Fluorescence Analysis Methods
