This standard specifies the determination principle, operation steps, result calculation and method precision of boron in uranium dioxide pellets. This standard is applicable to the determination of boron in uranium dioxide cakes and also to the determination of boron in nuclear linear triuranium octoxide. GB/T 11839-1989 Determination of boron in uranium dioxide pellets Curcumin extraction photometry GB/T11839-1989 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Determination of boron in uranium dloxide pellets-The curcumin extractian-Spectrophotometric method
Subject content and scope of application
GB 11839-89
This standard specifies the determination principle, operating steps, result calculation and method precision of boron in uranium dioxide pellets. This standard is applicable to the determination of boron in uranium dioxide pellets and also to the determination of nuclear-grade triboron octoxide. The sampling amount is 0.500g. Determination range: Uranium monoxide boron content is 0.1-1.0 μg/g2 Method: The sample is dissolved in concentrated sulfuric acid and hydrogen peroxide. After dehydration and defluorination, boron and curcumin form a red complex in the aqueous medium of sulfuric acid and glacial acetic acid. After dilution with water, it is extracted with cyclohexanone solution containing phenol and the organic phase is filtered. At a wavelength of 560nm on the spectrophotometer, the cyclohexanone solution containing phenol is used as a reference solution to measure its absorbance. The microgram amount of coexisting elements allowed per gram of sample is PO}- (1000), Ni (150), F (120), Cr (100), Mo (100), V (100), Ti (100), Si (100) + Zr (100), Sn (100), Cu (100), Ca (10n), Mn (50), Vb (40), Ta (30); the interference of Fe is eliminated with sulfuric acid hydrogenation. 3 Reagents
Unless otherwise specified, analytical reagents that meet national standards were used during analysis. 3.1 Hydrogen peroxide (CH3COCl3) 99.5%
8.2 Hydrogen peroxide (H2O2) 30%: 3.3 High-purity water
Purification method: Place ion exchange water in a quartz distillation tower or quartz azeotropic distillation, add a small amount of glycol, and store it in a polyolefin bottle after distillation:
3.4 ​​Glacial acetic acid (CH3COCl3) 17.4mol/L Purification method: Add 5ml of glacial acetic acid to a quartz distiller, and add 1000mL of glacial acetic acid in an aqueous solution containing 0.4g/mL glycol. Place in leaf oil braid and steam, remove 10% of the initial fraction, and take 70% of the fraction in a flask; 3.5 sulfuric acid (H2SO4) pure, 17.8ml/1, purification method: add 60mL sulfuric acid to the platinum dish, slowly add 30mL fluoric acid (superior pure) with a polyethylene pipette, stir with a platinum sheet, heat on a 1000W electric furnace and place in a concentrated oven, remove and cool, and repeat the above operation. After cooling, transfer to a flask 3.6 sulfuric acid hydrazine (HN·NHz·HSO4) solution 1.0% (m/V) weigh 0.5g of alkaline acid hydrazine and place in a platinum dish, add 25mL sulfuric acid (3.5), and dissolve at low temperature on an electric furnace. Transfer to a 50mL quartz volumetric plate, dilute to scale with sulfuric acid (3.5), 3.7 Curcumin (C21HzO)
Purification method: weigh 5g of curcumin and place it in a 250mL beaker [1, add 150mL of a mixture of acetone and high-purity water (2+1) State Technical Supervision Bureau 1989-10-21 approved 1990-08-01 implementation
GB11839-89
dissolve, filter, and place the filtrate in the beaker for 2h. Wash the product with high-purity water (3,). Transfer the crystals into a quartz beaker, cover with quartz surface, bake in an oven at 10℃ for about 6h, then transfer to a polyethylene bottle for storage. 3.B Curcumin solution 0.1% (m/V) z
Weigh 0.05Ug curcumin (3.7) into a 200mL poly/ethylene bottle!, add 50mL ice/liquid (3.4) to dissolve 8.9% (C!,0H)-cycloL ECH(CH)CO1 benzene (1.0%) (m/V): Weigh 5.0g phenol and dissolve in 500ml cyclohexanone: 3.10 Standard wide storage solution Weigh 0.5720g boric acid (spectrally pure) and place in a 1000mL quartz container. Add high-purity water (3.3) to dissolve and dilute to the scale, shake to hook. 1 mL of this solution contains 10% boron; 3.11 Boron Standard Solution Pipette 5.0 mL of the boron standard stock solution (3.10) into a 500 mL quartz container, and dilute to scale with high-purity water (3.3), shake well. 1 mL of this solution contains 1.0 μ boron. 4.1 Spectrophotometer wavelength range 360-800mm14.2 Put a layer of cotton cloth on the electric heating plate and adjust the temperature to 100-130℃ at the lowest point and 180-220℃ at the highest point by using the transmitter4.3 Quartz distillation or quartz distiller:4.4 Quartz distiller 1000mL;4.5 Platinum nozzle 100mL;4.6 Pear-shaped liquid separator 1MomL;4.7 Analytical sensitivity 0.1mg:4.8 Sieve diameter 0.074mm, made of polyethylene.5 Samples5.1 Sampling principlesThe collection and packaging process of samples must ensure that the specific components and characteristics to be separated do not change. The collected samples must have representative columns.
5.2 Sample preparation
Grind the sample into powder with a mortar, pass all of it through a polyethylene filter (4.8), and store it in a polyethylene bottle. 5.3 Sample volume
The sample volume should be no less than 3 times the sample volume for determination
6 Analysis steps
6.1 Sample analysis
6.1.1 Weigh 0.500 ml of sample, put it into a 30 mL quartz cup, add 1.0 mL sulfuric acid (3.5), and 3.0 mL hydrogen peroxide (3.2) and mix well. Cover with 1 quartz glass.
6.1.2 Dissolve the sample in a low temperature place on a hot plate (4.2), and remove the molten salt. Move to the electric hot plate (4.2) and heat for 2-3 minutes. The volume is controlled at about 1.8 mL. When the smoke is gone, add 1.5 mL of glacial acetic acid (3.4) immediately and mix. Place in a 25°C water bath and add 3.0 mL of curcumin solution (3.8) and mix. Add 0.5 mL of hydrazine sulfate solution (3.6) and mix. Incubate in a 18=2°C water bath for 30 minutes.
6.1.4 Transfer the solution to a 10 μL separatory tube + tH2O (3.3) and dilute to 45+3 mL. Add 10 mL of benzene powder-cyclohexanone extractant (3.9) and extract by shaking for 1 minute. Dephase after about 10 minutes. 6.1.5 Transfer the organic phase to a 10 mL volumetric flask, rinse the separatory tube with acetone (3.1) and mix the rinsed acetone with the organic phase, dilute to the mark with acetone (3.1), and mix for about 2 minutes. Filter with double-layer filter paper 6.1.6 "Measure the absorbance at a wavelength of 5601 nm on the spectrophotometer, using 1 cm colorimetric solution and phenol-cyclohexane extractant (3.9) as reference solution.
6.2 Determination of reagent blank
GB 118398
6.2.1 Add 1.0mL of ethanol (3.5) and 3.0mL of peroxide (3.2) to a 30mL quartz beaker and mix. Evaporate on a hot plate (4.2) until a little smoke appears for 2-3 minutes and control the volume to about 0.8mL. Remove. Follow the steps 6.1.3 to 6.1.6. 6.3 Drawing of working curveWww.bzxZ.net
6.8.1 Transfer 0.000, 0.050, 0.100, 0.200, 0.300, 0.400, and 0.500mL of boron standard solution (3.11) to seven 30mL quartz beakers respectively. Add 0 .500 ml of potassium oxide matrix with a boron content of less than 0.050 μ/g, 1.0 nL sulfuric acid (3.5), 3.0 mL hydrogen peroxide (3.2), mix well. Cover 1 quartz surface with blood. The following operations are performed according to 6.1.2 to 6.1.6. Use the absorption as the horizontal axis and the net absorbance as the vertical axis to draw a working curve. Result calculation
Where: C is the content of small boron in the sample, g/g: A is the boron content of the net absorbance measured on the working curve, Hm~ is the mass of the measured sample, g.
8 Method precision
Water value m
Repeatability r
Reproducibility R
GB 11839—89
Appendix A
Precautions for using this standard
(Supplement)
A1 The total blank of sulfuric acid, glacial acetic acid, hydrazine sulfate solution, curcumin solution, hydrogen peroxide and high-purity water must be less than 0.040g boron. A2 The 30mL quartz beaker should be soaked with ion exchange water after each use. Before use, it must be heated and boiled with concentrated sulphuric acid, and then washed with ion exchange water and high-purity water (3.3). The quartz beaker should be placed upside down on filter paper and the water in the quartz beaker should be dripped dry. A The curcumin solution (3.8) should not be left for more than 12h. A4 If the sample is not completely dissolved after adding 3.0mL hydrogen peroxide (3.2), hydrogen peroxide (3.2) until the sample is completely dissolved.
A5 laboratories must be wet cleaned, and the fume hood must be covered with a plastic plate or plexiglass plate. All operations before extraction must be performed in a fume hood.
Additional remarks:
This standard was proposed by China National Nuclear Corporation. This standard was drafted by the State-owned 813. This standard was drafted by Li Junhua.
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