Skip to product information
1 of 10

PayPal, credit cards. Download editable-PDF and invoice in 1 second!

JC/T 1088-2008 English PDF (JCT1088-2008)

JC/T 1088-2008 English PDF (JCT1088-2008)

Regular price $150.00 USD
Regular price Sale price $150.00 USD
Sale Sold out
Shipping calculated at checkout.
Quotation: 24-hr self-service. Click JC/T 1088-2008
See Chinese contents: JC/T 1088-2008

JC/T 1088-2008: Methods for chemical analysis of granulated electric furnace phosphorous slag

This standard specifies the benchmark method and substitution method for the method of chemical analysis of granulated electric furnace phosphorus slag. In case of dispute, the benchmark method shall prevail. This standard applies to the granulated electric furnace phosphorus slag used in the building materials industry and other materials designated to adopt this standard.
JC/T 1088-2008
BUILDING MATERIAL INDUSTRY STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
ICS
Registration number: 24205-2008
Methods for chemical analysis of granulated
electric furnace phosphorus slag
ISSUED ON: JUNE 16, 2008
IMPLEMENTED ON: DECEMBER 01, 2008
Issued by: National Development and Reform Commission of PRC
Table of Contents
Foreword ... 4
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 5
4 Basic requirements of test ... 6
5 Reagents and materials ... 7
6 Instruments and equipment ... 12
7 Preparation of specimen ... 13
8 Determination of loss on ignition - Ignition reduction method ... 13 9 Determination of silica - Potassium fluorosilicate capacity method ... 14 10 Determination of ferric oxide - EDTA direct titration ... 14
11 Determination of aluminum oxide - EDTA direct titration ... 14
12 Determination of calcium oxide - Calcium carbonate back titration ... 14 13 Determination of magnesium oxide - Atomic absorption spectroscopy
(reference method) ... 16
14 Determination of sulfur trioxide - Barium sulfate gravimetric method ... 16 15 Determination of potassium oxide and sodium oxide - Flame photometric method ... 16
16 Determination of phosphorus pentoxide - Ammonium phosphomolybdate
colorimetric method ... 16
17 Determination of magnesium oxide - EDTA titration reduction (substitution) ... 17
18 Determination of fluoride ions - Ion selective electrode method ... 18 19 Determination of chloride ions - Phosphoric acid distillation - Mercury salt titration ... 18
20 Repeatability limits and reproducibility limits ... 19
Foreword
The consistency between this standard and EN 196-2:2005 ?€?Method of testing cement - Part 2: Chemical analysis of cement?€? and ASTM C114:2005 ?€?Standard test methods for chemical analysis of hydraulic cement?€? is not equivalent. This standard was proposed by the China Building Materials Federation.
This standard shall be under the jurisdiction of the National Cement
Standardization Technical Committee (SAC/TC 184).
Drafting organizations of this standard: China Building Materials Science Research Institute, China Building Materials Inspection and Certification Center. Main drafters of this standard: Yan Weizhi, Wang Ruihai, Wang Guanjie, Wen Yugang, Huang Xiaolou.
This standard is the first release.
Methods for chemical analysis of granulated
electric furnace phosphorus slag
1 Scope
This standard specifies the benchmark method and substitution method for the method of chemical analysis of granulated electric furnace phosphorus slag. In case of dispute, the benchmark method shall prevail.
This standard applies to the granulated electric furnace phosphorus slag used in the building materials industry and other materials designated to adopt this standard.
2 Normative references
The provisions in following documents become the provisions of this standard through reference in this standard. For the dated references, the subsequent amendments (excluding corrections) or revisions do not apply to this standard; however, parties who reach an agreement based on this standard are
encouraged to study if the latest versions of these documents are applicable. For undated references, the latest edition of the referenced document applies. GB/T 176-2008 Methods for chemical analysis of cement
GB/T 2007.1 General rules for the sampling and sample preparation of
minerals in bulk - Sampling by manual method
GB/T 6682 Water for analytical laboratory use - Specification and test
methods
3 Terms and definitions
The terms and definitions as established in the GB/T 15000 series as well as the following terms and definitions apply to this standard.
3.1
Repeatability conditions
The conditions for independent test of the same tested object in the same laboratory, by the same operator using the equipment, according to the same test method, in a short period of time.
3.2
Reproducibility conditions
The conditions for independent test of the same tested object in different laboratories, by different operators using different equipment, according to the same test method.
3.3
Repeatability limit
A value, under the repeatability conditions (3.1), the probability that the absolute difference between the two test results is less than or equal to this value is 95%.
3.4
Reproducibility limit
A value, under reproducibility conditions (3.2), the probability that the absolute difference between the two test results is less than or equal to this value is 95%.
4 Basic requirements of test
4.1 Number of tests and requirements
The number of tests per determination is specified as two. Use the average value of the two tests to express the determination result.
Before the analysis, the specimen shall be baked at 105 ??C ~ 110 ??C for 2 h, cooled to room temperature in a desiccator, then weighed.
In the chemical analysis, unless otherwise stated, it must determine the loss on ignition at the same time. For other determinations, it shall carry out the blank test at the same time, meanwhile correct the test results.
4.2 Expression of mass, volume, results
Use ?€?grams (g)?€? to express mass, accurate to 0.0001 g. The burette?€?s volume is expressed in ?€?milliliter (mL)?€?, accurate to 0.05 mL. The unit of titer is expressed in ?€?milligram per milliliter (mg/mL)?€?.
The titer of chloride ions in the standard titration solution of mercury nitrate retains three significant digits after the rounding off. The titer and volume ratio of other standard titration solutions retain four significant digits after the rounding off.
Unless otherwise stated, the results of each analysis are based on mass fraction. The analytical results of the chloride ion are expressed in % to three decimal places. The analytical results of other items are expressed in % to two decimal places.
4.3 Blank test
Use the same amount of reagent. Do not add specimen. Use the same
determination procedures to carry out test, to correct the determination results as obtained.
4.4 Ignition
Place the filter paper and the precipitate in a crucible which has previously been burned to a constant weight. To avoid producing flame, in an oxidizing
atmosphere, slowly dry and ash it. After ashing it to the absence of black carbon particle, then place it in a high-temperature furnace (6.4), to burn it at the specified temperature. In a desiccator (6.3), cool it to room temperature. Weigh it.
4.5 Constant weight
After the first burning, cooling, weighing, use the method of applying continuous burning of 15 min, cooling, weighing, to check the constant mass. When the difference between two consecutive weighing results is less than 0.0005 g, it reaches constant weight.
5 Reagents and materials
Unless otherwise stated, the reagents used shall be not less than analytical pure. The water used shall meet the requirements for grade-3 water as
specified in GB/T 6682.
The density of commercially available concentrated liquid reagents as listed in this standard refers to a density (??) at 20 ??C, in grams per cubic centimeter (g/cm3). In chemical analysis, the acid or ammonia used, unless otherwise the concentration is not indicated, refers to commercially available concentrated acid or concentrated ammonia. Use the volume ratio to indicate the degree of dilution of the reagent. For example, hydrochloric acid (1 + 2) means that 1 part by volume of concentrated hydrochloric acid is mixed with 2 parts by volume of water.
5.1 Hydrochloric acid (HCI)
1.18 g/cm3 ~ 1.19 g/cm3, mass fraction 36% ~ 38%.
5.2 Hydrofluoric acid (HF)
1.15 g/cm3 ~ 1.18 g/cm3, mass fraction 40%.
5.3 Sulfuric acid (H2SO4)
1.84 g/cm3, mass fraction 95% ~ 98%.
5.4 Triethanolamine [N(CH2CH2OH)3]
1.12 g/cm3, mass fraction 99%.
5.5 Hydrochloric acid (1 + 1); (1 + 10)
5.6 Sulfuric acid (1 + 1)
5.7 Triethanolamine (1 + 2)
5.8 Sodium hydroxide (NaOH)
5.9 Anhydrous sodium carbonate
Use an agate mortar to grind the anhydrous sodium carbonate (Na2CO3) finely ground to a powder form.
5.10 Sodium carbonate-borax mixed flux (2 + 1)
Mix 2 parts by mass of anhydrous sodium carbonate (Na2CO3) and 1 part by mass of anhydrous borax (Na2B4O7) uniformly and grind it finely. Store it in a sealed bottle.
5.11 Sodium hydroxide solution (200 g/L)
Dissolve 20 g of sodium hydroxide (NaOH) in water. Add water to dilute it to 100 mL. Store in plastic bottles.
5.12 Potassium hydroxide solution (200 g/L)
Dissolve 200 g of potassium hydroxide (KOH) in water. Add water to dilute it to 1 L. Store in plastic bottles.
5.13 Ammonium molybdate solution (15 g/L)
Dissolve 3 g of ammonium molybdate [(NH4)6Mo7O24 ?€? 4H2O) in 100 mL of hot water. Add 60 mL of sulfuric acid (1 + 1) and shake it uniformly. After cooling, add water to dilute it to 200 mL. Store the solution in a plastic bottle. This solution is used within one week.
5.14 Ascorbic acid solution (50 g/L)
Dissolve 5 g of ascorbic acid (V.C) in 100 mL of water. If necessary, filter it before use. Prepare it before use.
5.15 pH10 buffer solution
Dissolve 67.5 g of ammonium chloride (NH4Cl) in water. Add 570 mL of
ammonia water (NH3 ?€? H2O). Add water to dilute it to 1 L.
5.16 Sodium potassium tartrate solution (100 g/L)
Dissolve 10 g of sodium potassium tartrate (C4H4KNaO6 ?€? 4H2O) in water. Add water to dilute it to 100 mL.
5.17 Potassium fluoride dissolution (20 g/L)
Dissolve 20 g of potassium fluoride (KF ?€? 2H2O) in water. Add water to dilute it to 1 L. Store it in a plastic bottle.
5.18 Preparation of phosphorus pentoxide (P2O5) standard solution
5.18.1 Preparation of phosphorus pentoxide standard solution
Weigh 0.1917 g of potassium dihydrogen phosphate (KH2PO4, reference
reagent) which has been baked at 105 ??C ~ 110 ??C for 2 h, accurate to 0.0001 g. Place it in a 300 mL beaker. Add water to dissolve it. Transfer it in a 1000 mL volumetric flask. Use water to dilute it to the mark. Shake it uniformly. Each milliliter of this standard solution contains 0.1 mg of phosphorus pentoxide. Pipette 50.00 mL of the above standard solution into a 500 mL volumetric flask. Use water to dilute it to the mark. Shake it uniformly. Each milliliter of this standard solution contains 0.01 mg of phosphorus pentoxide.
5.18.2 Drawing of working curve
Pipette 0 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL, 15.00 mL, 20.00 mL, 25.00 mL of standard solution which contains 0.01 mg of phosphorus
pentoxide per ml into a 200 mL beaker. Add water to dilute it to 50 mL. Add 10 mL of ammonium molybdate solution (5.13) and 2 mL of ascorbic acid solution (5.14). Heat to slightly boil it for (1.5 ?? 0.5) min. After cooling it to room temperature, transfer it in a 100 mL volumetric flask. Use hydrochloric acid (1 + 10) to rinse the beaker. Use hydrochloric acid (1 + 10) to dilute it to the mark. Shake it uniformly. Use a spectrophotometer and 10 mm cuvette to determine the absorbance of the solution at a wavelength of 730 nm, which uses water as a reference. Use the determined absorbance as a function of the corresponding phosphorus pentoxide content, to draw the working curve.
5.19 Calcium carbonate standard solution [c(CaCO3) = 0.024 mol/L]
Weigh 0.6 g (m1) of calcium carbonate (CaCO3, reference reagent) which has been baked at 105 ??C ~ 110 ??C for 2 h, accurate to 0.0001 g. Place it in a 400 mL beaker. Add about 100 mL of water. Cover the watch glass. Slowly add 5 mL ~ 10 mL of hydrochloric acid (1 + 1) along the mouth of the beaker. Stir it until all the calcium carbonate is dissolved. Heat the solution to boil. Cool it to room temperature. Transfer it in a 250 mL volumetric flask. Use water to dilute it to the mark. Shake it uniformly.
5.20 EDTA standard titration solution [c(EDTA) = 0.015 mol/L]
5.20.1 Preparation of EDTA standard titration solution
Weigh about 5.6 g of EDTA (ethylene diamine tetraacetic acid, C10H14N2O8Na2 ?€? CHO) in a beaker. Add about 200 mL of water. Heat it to dissolve it. Filter it. Add water to dilute it to 1 L. Shake it uniformly.
5.20.2 Calibration of EDTA standard titration solution?€?s concentration
Pipette 25.00 mL of calcium carbonate standard solution (5.19) into a 400 mL beaker. Add water to dilute it to about 200 mL. Add appropriate amount of CMP mixing indicator (5.22). Whilst stirring it, add potassium hydroxide solution (5.12) until green fluorescence appears. Add another 2 mL ~ 3 mL. Use EDTA
standard titration solution to titrate it until the green fluorescence disappears and red appears.
The concentration of the EDTA standard titration solution is calculated according to formula (1):
Where:
c(EDTA) - The concentration of the EDTA standard titration solution, in moles per liter (mol/L);
V1 - The volume of the EDTA standard titration solution as consumed in
titration, in milliliters (mL);
m1 - The mass of calcium carbonate in the calcium carbonate standard
solution as prepared in accordance with 5.19, in grams (g);
100.09 - The molar mass of CaCO3, in grams per mole (g/mol).
5.20.3 Calculation of titration of each oxide by EDTA standard titration solution
The titer of EDTA standard titration solution for ferric oxide, aluminum oxide, calcium oxide, magnesium oxide is calculated according to formula (2), formula (3), formula (4), formula (5), respectively:
Where:
TFe2O3 - The titer of EDTA standard titration solution for ferric oxide, in milligrams per milliliter (mg/mL);
TAl2O3 - The titer of EDTA standard titration solution for aluminum oxide, in milligrams per milliliter (mg/mL);
TCaO - The titer of EDTA standard titration solution for calcium oxide, in milligrams per milliliter (mg/mL);
TMgO - The titer of EDTA standard titration solution for magnesium oxide, in milligrams per milliliter (mg/mL);
c(EDTA) - The concentration of the EDTA standard titration solution, in moles per liter (mol/L);
79.84 - The molar mass of (1/2Fe2O3), in grams per mole (g/mol);
50.98 - The molar mass of (1/2Al2O3), in grams per mole (g/mol);
56.08 - The molar mass of CaO, in grams per mole (g/mol);
40.31 - The molar mass of MgO, in grams per mole (g/mol).
5.21 Calcium carbonate standard titration solution [c(CaCO3) = 0.015
mol/L]
5.21.1 Preparation of standard titration solution
Weigh 1.50 g of calcium carbonate (CaCO3) which has been baked at 105 ??C ~ 110 ??C for 2 h. Place it in a 400 mL beaker. Add about 200 mL of water. Cover the watch glass. Slowly add 5 mL ~ 10 mL of hydrochloric acid (1 + 1) along the mouth of beaker. Stir it until all the calcium carbonate is dissolved. Heat to boil it for several minutes. Cool the solution to room temperature. Transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Shake it uniformly. 5.21.2 Calibration of volume ratio of EDTA standard titration solution to calcium carbonate standard titration solution
Slowly release 10 mL ~ 15 mL EDTA standard titration solution (5.20) from the burette into a 400 mL beaker. Add about 200 mL of water. Add appropriate amount of CMP mixing indicator (5.22). Whilst stirring it, add potassium hydroxide solution (5.12) until a stable red color appears. Add another 2 mL ~ 3 mL. Use calcium carbonate standard titration solution (5.21.1) to titrate it until a green fluorescence appears.
The volume ratio of the EDTA standard titration solution to the calcium carbonate standard titration solution is calculated according to formula (6): Where:
K1 - The volume ratio of EDTA standard titration solution to calcium
carbonate standard titration solution;
V2 - The volume of the EDTA standard titration solution, in milliliters (mL); V3 - The volume of the calcium carbonate standard titration solution as consumed in titration, in milliliters (mL).
5.22 Calcein - methyl thymol blue - phenolphthalein mixed indicator
(shortly referred to as CMP mixed indicator)
Weigh 1.000 g of calcein, 1.000 g of methyl thymol blue, 0.200 g of
phenolphthalein, 50 g of potassium nitrate (KNO3) which has been dried at 105 ??C ~ 110 ??C. Mix and grind it fine. Store it in a mouth-grinding bottle. 5.23 Acid chrome blue K - naphthol green B mixed indicator (shortly
referred to as KB mixed indicator)
Weigh 1.000 g of acid chrome blue K, 2.500 g of naphthol green B, 50 g of potassium nitrate (KNO3) which has been dried at 105 ??C ~ 110 ??C. Mix and grind it fine. Store it in a mouth-grinding bottle.
5.24 P-nitrophenol indicator solution (2 g/L)
Dissolve 0.2 g of p-nitrophenol in 100 mL of water.
6 Instruments and equipment
6.1 Balance
It shall not be lower than grade-4, accurate to 0.0001 g.
6.2 Platinum, silver, porcelain crucible
It has a lid. The capacity is 15 mL ~ 30 mL.
6.3 Dryer
It is loaded with color-changing silica gel.
6.4 High-temperature furnace
For the flame-isolated heating furnace, carry out resistance heating on the periphery of the furnace. It shall use temperature controller to accurately control the furnace?€?s temperature. The controllable temperature is (950 ?? 25) ??C. 6.5 Glass capacity vessel
Burette, volumetric flask, pipette.
6.6 Spectrophotometer
It can, within the range of 400 nm ~ 800 nm, determine the absorbance of the solution. It is equipped with a 10 mm cuvette.
7 Preparation of specimen
Use the method of GB/T 2007.1 to take sample. The samples as sent to the lab shall be representative uniform samples. Use quartering method or a reducer to reduce the specimen to about 100 g. Use a 80 ??m square-hole sieve to sieve it. Use a magnet to remove the metal iron from the materials as left on the sieve. Grind the materials as left on the sieve to make it all pass a 80 ??m square-hole sieve. Thoroughly mix it uniformly. Contain it in the sample bottle. Seal it for preservation, to prepare for determination.
8 Determination of loss on ignition - Ignition reduction
method
8.1 Summary of method
The specimen is burned in a high-temperature furnace at (950 ?? 25) ??C, to drive off carbon dioxide and moisture, while oxidizing the existing oxidizable elements.
8.2 Analytical procedures
Weigh about 1 g of specimen (m2), accurate to 0.0001 g. Place it in a porcelain crucible which has been burned to constant weight. Place the lid inclined on the crucible. Place it in a high-temperature furnace (6.4). From low temperature, gradually increase the temperature. Burn it at (950 ?? 25) ??C for 15 min ~ 20 min. Remove the crucible to place it in a desiccator (6.3). Cool it to room temperature. Weigh it. Repeat burning, until reaching to constant weight.
8.3 Calculation and representation of results
The mass fraction of the loss on ignition wLOI is calculated according to formula (7):
Where:
wLOI - The mass fraction of loss on ignition, %;
m2 - The mass of sample, in grams (g);
m3 - The mass of sample after burning, in grams (g).
9 Determination of silica - Potassium fluorosilicate
capacity method
It is carried out according to clause 23 of GB/T 176-2008.
10 Determination of ferric oxide - EDTA direct titration
It is carried out according to clause 12 of GB/T 176-2008.
11 Determination of aluminum oxide - EDTA direct
titration
It is carried out according to clause 13 of GB/T 176-2008.
12 Determination of calcium oxide - Calcium
carbonate back titration
12.1 Summary of method <...

View full details