HG/T 2956.6-2001 Determination of calcium oxide and magnesium oxide content in boron and magnesium ores - Volumetric method
Some standard content:
1cs 73.080
Chemical Industry Standard of the People's Republic of China
HG/T 2956.2~2956.82001
Analytical methods for ascharite ores2002-01-24Promulgated
2002.0701Implementation
Promulgated by the State Economic and Trade Commission
Requisition No.: 10103-2002
IG/T2956.6—2001
This standard is a recommended chemical industry standard [IG/T2U55.5-1082] for the analysis of ascharite ores containing calcium oxide and calcium oxide.
This standard is issued by the National Chemical Industry Policy and Regulations Department of Beijing, and is the same as the standard HG/1'2956.51982. This standard is issued by the Chemical Industry Chemical Standardization Technical Committee, Yekou. The responsible drafting unit of this standard is Lianyungang Institute of Chemical Industry. The main drafters of this standard are Yi Heban and Zhang Conghai. This standard was first issued in 1066. The Ministry of Chemical Industry issued the standard IG_-32-6 for the first time. It was issued in 102 as the national standard G147.G-2 for the analysis of calcium oxide and magnesium content in magnesium ore. 3,159? It was adjusted to a recommended chemical industry standard in 2000, with the new number of IIGT2956.6 [S8219]. 1 Scope Chemical Industry Standard of the People's Republic of China Determination of calcium oxide and magnesium axides content in magnesium ore Volumetric method Asclinrile ore Determination of calcium oxide and magnesium axides content Volumetric method This standard specifies the determination of calcium oxide and magnesium axides content: This standard is applicable to the determination of calcium oxide and magnesium oxide content in magnesium ore products. 2 Reference standards HG/T2956.6—2001 HP/T 2355. 5—1182
The following provisions are covered by the standard and are used as the final standard in this standard. When this standard is issued, the version shown is valid. All standards will be revised. Parties using this standard should use the latest version of the following standards as soon as possible. GB/T 601-1H9 Chemical reagents for quantitative analysis (volume analysis) Preparation of standard reagents/6621932 New laboratory water test method (02G921 [987) 3 Method Summary
The sample is decomposed with hydrochloric acid and fluorinated chain. In the H value of 12.59, With acid K+3 as indicator, FGTA standard titration can determine calcium, pH 8.0 and other low levels of nitrite, with FLTA decalcification, with acid K+3 as indicator. With EDTA standard titration solution, CITA standard titration solution can determine magnesium. 4 Reagents and solutions
The water used in this standard should comply with (5/T5582 medium-grade water, listed reagents. Except for those specified, all reagents are analytically pure. 4.1 Ammonium hydroxide.
4.2 Salt monohydrate: 1--
4.3 Tide filter: 3FgT. || tt||Weigh the 3 phases and dissolve them in 100 boiling water, cool
4.4.7. Alcohol amine solution: add 4.
4.5 Potassium oxide solution: J2/1.
4.6 Ammonia-ammonium chloride solution (II=10). Weigh 67.5g of chlorinated water and add 70ml of natural water, dilute with water to 10m, shake well. 4.77. Dichloroethylene diamine acetic acid (EGTA) standard solution: (FGTA)=0.01H01/14.7.1 Preparation
Weigh 3.5g of FGTA in 20cmI Add potassium hydroxide to water and add until completely dissolved. Dilute to 100 mL with water. 4.7.2 4.7.2.1 Calcium hydroxide standard solution, e(Ca)=U.1uwl/1 Approved by the National Economic and Trade Commission on January 24, 2002 and implemented on July 1, 2002 HG/I2956.6—2001 Take 1.00088125--110℃ dried to decomposition (standard reagent) and place in 13 ml of 4% ethanol. Remove carbon dioxide from the bottle and dilute with water until 20 minutes, shake for 3 minutes. 4.7.2.2 Use an isocratic tube to draw 10.1 ml of the standard oxygen standard solution, add 10% ml of water, ≤4 ml of magnesium oxide standard concentrate (4.8. 2, 11, 15 ml of the concentrate, 5 ml of ethanol gel sieve, and remove the hook. Add 10 mT potassium hydroxide solution, 1.5 ~ 5% clear acid chrome blue K case phenol green R indicator solution (4.10), and use ETA rate to titrate the whole crushed sieve to a bright blue color as the end point: At the same time, perform a blank test. 4.7.2.3 The titration of the EGTA standard titration solution is calculated using the formula (:), (EGTA) =
Where: r(EGTA)
The titration of the EGTA standard titration solution is maL/T.! The titration of the calcium-based non-free solution is mnl/IF
Calcium ionization rate: approx. 1 mL: volume of cold standard solution A. 0.01 mL 4.8 Disodium ethylenediaminetetraacetic acid (EDTA) standard solution: tc(EDTA) = U.02 mol/L 4.8.1 Prepare 1 mL FDA water and dilute to 1 mol/L 4.8.2 Calibration 4.8.2. 1 Oxidation standard solution: c(MgO) 0.02 sl/L, (1)
Take 10ml of 1-3 aldehyde solution in S3C and transfer it to a 100nm volumetric flask. Dilute with water to the mark. Add 23.5ml of magnesium oxide standard solution with a pipette. Add 100ml of water and 5ml of triethylamine solution. Add 10aL of ammonia·chlorine solution, 4-5 drops of acidic blue K-distillate (1.11), and moisten with EDTA until a slight blue-green color is obtained. At the same time, do a short test. 4.8.2. 3F1YA standard titration solution is calculated according to formula 2), c,w
r(EDTA)=-V
Wu: c(EDTA)
EYIA standard titration solution liquid density, MI/IR chemical lock solution density, mO./L:
single chain standard volume·mL; Www.bzxZ.net
EDTA standard titration solution volume·mI;
V-vacuum test EDTA standard calibration solution volume, mI.4.92,2-cyclohexane-4-Z waist (CDTA> standard titration solution: c(CDTA)=U.Uet/L4. 9. 1 Preparation
Weigh 7% ClA in 200mL water. Add potassium hydroxide dropwise until completely dissolved. Dilute with water to 100 cal. 4.9.2 Calibration
Calibrate and calculate according to 4.8.2.2 to 4.8.2.3. 4.10 Acid K-phenol B indicator solution.
Take 0.15% chromium blue K.15% chromium green H.15% and mix it in 50mL water (the useful life is two weeks). 4.11 Acid K-phenol B indicator solution. Weigh 0.3g chromium blue K.15% chromium green H.15% and mix it in 50mL water (the useful life is two weeks). 5 Sample
The sample passes through a 125um test sieve (G/0.10 Ca.). Place it in a desiccator at 10-110°C and cool to room temperature. 22
6 Analytical steps
6.1 Preparation of test sample
[IG/T 2956.6-2001
Weigh 0.2g of sample (minimum 0.0002g), put it into a small dish of water, add 12-15L salt solution, about 1 bottle of hydrogen peroxide, heat on the hot plate until the sample is completely decomposed, heat it to 3~bm, cool it below the surface, transfer it to a 150m volumetric flask, dilute it with water to the scale, and list it. 6.2 Determination of calcium oxide
Pick up 20.0ml of test sample, put it into a 250ml washing cup, add 100ml of water, 15ml of ethanol solution, 5ml of triethanolamine solution, stir it, and add 1ml of potassium peroxide solution to make the pH value of the solution greater than 12.5. Add 4-5 parts of acidic K-green B solution and use FTA marker to determine the point at which the secretion is completely condensed and the blue negative is the drop point.At the same time, start the short test:
6.3 Set of magnesium chloride test
Collect 20.0mL test tube, add 250mL of water, 100ml of triethanolamine solution, stir with a spoon. Add 11ml of aqueous hydrogen peroxide buffer, then add 0.51mL of EGTA standard solution more than the titration emulsification solution, 4-5 drops of acid blue K-green B-yellow indicator + EITA standard solution or CTA standard titration solution. The titration solution turns green as the end point.
Make a timer in the room. You can use a 2-mg oxygenated gas to calibrate the time of the titration. Add 2*mg of the gas. 3 drops, if the temperature is lower than 15, the trap solution needs to be heated by 3℃ to facilitate the establishment of the correct 7. Expression of analytical results
7.1 Calcium oxide (Ca) content
Calcium oxide (C) content expressed in mass percentage () is calculated according to formula [3): X -c(v,-V2a 056.u8x100
Wherein.
Actual concentration of EGTA standard titration solution, nn./L; Volume of HGTA standard titration solution, ml
Volume of blank EGTA standard titration solution, ml. The mass of the most suitable titration solution,
The mass of calcium oxide in grams equivalent to mLA standard titration solution LEGTA=1,000/:
7.2 Magnesium oxide (MO) content
Oxide (MuO\) content expressed as mass percentage (X: Calculated by formula (4): X: -V.Ve3XU. 040-1x1G3
Where: c
actual capacity of EDTA standard moistening solution, ImE/L: volume of EDTA standard titration, mL
change to the volume of FDTA standard titration solution. mT: suction capacity is equivalent to the test air volume, P
is equivalent to 1.00mI.HITA standard solution [c(EDTA-1.00Gmnl/L] is the mass of magnesium oxide expressed in grams.
8 allowable difference
HG/I 2956. 6—2001
The arithmetic mean of the results of the parallel analysis was taken as the most complete analysis detail, and the initial difference of the analysis results of the same laboratory and the absolute difference of the analysis results of different laboratories were not much different as shown in Table 1. Table 1 The results of the same laboratory and different laboratories were
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