CN102432069A - Process for preparing standard substance of nonmetallic elements for biuranate - Google Patents
Process for preparing standard substance of nonmetallic elements for biuranate Download PDFInfo
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- CN102432069A CN102432069A CN2011102742163A CN201110274216A CN102432069A CN 102432069 A CN102432069 A CN 102432069A CN 2011102742163 A CN2011102742163 A CN 2011102742163A CN 201110274216 A CN201110274216 A CN 201110274216A CN 102432069 A CN102432069 A CN 102432069A
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Abstract
The invention discloses a process for preparing a standard substance of nonmetallic elements for biuranate, which comprises the steps of: at first, performing co-precipitation of phosphorus and silicon into the biuranate, wherein fluorine is partially co-precipitated into the biuranate by a precipitating and crystallizing method; and then synthesizing sulphur, chlorine and small part of fluorine into the biuranate by a slurrying evaporation method to prepare the standard substance which meets the magnitude of five nonmetallic impurity elements (sulphur, phosphorus, silicon, fluorine and chlorine) of fixed values in the biuranate. The process provided by the invention can be conveniently used to prepare the standard substance of nonmetallic elements for the biuranate in different contents and the standard substance of nonmetallic elements for the biuranate prepared is consistent with the biuranate product produced by a uranium water smelting plant in physical properties.
Description
Technical field
The present invention relates to a kind of diuranate non-metallic element reference material preparation technology.
Background technology
The diuranate of uranium mill production at present all is sodium diuranate basically, and it is to be raw material with the uranium ore, selects acidleach or alkali soaking technology according to the raw material rerum natura, makes sodium diuranate with a series of chemical engineering unit operations such as ion exchange method or extraction processs then.Because foreign matter content is different in each uranium mill raw material; The technology condition of taking is also different; Sodium diuranate uranium grade and each impurity element index of producing also differ widely; For guaranteeing uranium purified product quality, diuranate each item element quality index has been made some regulations, promote each uranium mill that diuranate each item element quality index is tightened control.At present generally use the uranous uranic oxide reference material as quality control sample to the detection of diuranate each item impurity element; Because uranous uranic oxide reference material each item foreign matter content is low; Have difference on the rerum natura, some impurity index does not have, and needs to use standardized solution as quality control sample.
Summary of the invention
The object of the present invention is to provide a kind ofly can provide accurate detection, guarantees the preparation technology of the diuranate non-metallic element reference material of uranium purified product quality.
The preparation technology of this diuranate non-metallic element reference material provided by the invention comprises the steps:
(1). with the sodium diuranate is raw material, and sulphur, phosphorus, silicon, fluorine in this raw material, five nonmetallic impurity content of chlorine will be a little less than definite value nonmetallic impurity element amplitudes in the sodium diuranate;
(2). fully dissolve said raw material with analytical pure nitric acid, obtain lysate;
(3). the lysate that step (2) is obtained filters, and carries out liquid-solid separation, and the clear liquid constant volume that obtains after the separation is measured sulphur, phosphorus, silicon, fluorine, five non-metallic element content of chlorine and uranium content;
(4). the clear liquid behind the constant volume changes precipitation tank in term over to, stirs heating; When 40～60 ℃ of temperature, regulate acidity with sodium hydroxide solution, when the pH value is that 2～3 solution are when changeing muddy; Stop to add sodium hydroxide solution, after waiting to stir, in solution, add reagent; This reagent is the sodium hydroxide mark-on liquid mix reagent that contains phosphorus, silicon, fluorine element, with the phosphorus, silicon binomial element and the sodium diuranate co-precipitation that are difficult for being got off by water washing, and fluorine part and sodium diuranate co-precipitation; After adding whole reagent, controlling acidity is 6.0～7.0 in the pH value.Behind the molecular balance, continuing to add sodium hydroxide solution to acidity is 7.1～7.8 in the pH value, cooling cooling naturally, and whether phosphorus, silicon, fluorine content and uranium content reach in sampling monitoring analysis mother liquor of precipitation of ammonium and the crystal;
(5). cooled mother liquor of precipitation of ammonium of step (4) and crystal are used centrifugal filter centrifuging; Crystal is with after mother liquor of precipitation of ammonium is separated; Crystal with one-level water centrifuge washing, is removed wherein SODIUMNITRATE in whizzer, wherein the part fluorine element also washs from crystal;
(6). the sodium diuranate crystal after will washing is transferred to the baking oven inner drying, under 105 ℃～110 ℃, dries to constant weight;
(7). will dry to the sodium diuranate crystal of constant weight and grind, cross 100 order stainless steel sifts, send in the vortex mixer fully mixing then, and dry to constant weight again and accurately weigh, analyze sulphur, phosphorus, silicon, fluorine, cl content and uranium content;
(8). accurate weighing sulphur, fluorine, the plain add-on of chlorine trigram; Be prepared into solution; Stir in evaporating pan with the crystal powder after overground; Heating evaporation is blended into sulphur, phosphorus, chlorine trigram element in the diuranate through the slurrying method of evaporation, is evaporated to dry doubling and takes out 105 ℃～110 ℃ drying in oven to constant weight;
(9). step (8) is dried the sodium diuranate crystal regrinding to constant weight, cross 100 order stainless steel sifts, send into abundant mixing in the vortex mixer;
(10). the good sodium diuranate crystal of step (9) mixing is put into 105 ℃～110 ℃ drying in oven to constant weights obtain sample; Sample is through the homogeneity initial survey; The bottling and carry out uniformity testing qualified after, promptly make diuranate sulphur, phosphorus, silicon, fluorine, five non-metallic element reference materials of chlorine.
The present invention has set up diuranate nonmetallic impurity element reference material preparation technology; This process using liquid phase reaction, liquid phase blending manner; The reference material homogeneity effect of preparation is good; Process controllability is good, can conveniently prepare the diuranate nonmetallic impurity element reference material of different content, and the diuranate nonmetallic impurity element reference material that makes is consistent with the diuranate product rerum natura of uranium mill production.
Embodiment
Embodiment one
Prepare 30 kilopond uranium yellow non-metallic element reference materials, the value of definite value nonmetallic impurity element and expection uncertainty such as following table 1-1 in its sodium diuranate:
The value of definite value nonmetallic impurity element and expection uncertainty (%) in the table 1-1 sodium diuranate
| Element | S | P | Si | F | CL |
| Standard value | 3.0 | 1.0 | 1.5 | 0.3 | 0.5 |
| Combined standard uncertainty | 0.6 | 0.2 | 0.3 | 0.06 | 0.1 |
1. material dissolution
1.1 material is selected
Select sodium diuranate (barrel number 61-22) that certain ore deposit produces as raw material, its sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity constituent contents of chlorine and uranium and moisture content such as following table 1-2.
Table 1-2:
| Element (material) | S | P | Si | F | CL | U | H 2O |
| Content | 0.13% | 0.035% | 0.04% | <0.005% | 0.21% | 67.28% | 24.56% |
Require to select in the raw material sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity content of chlorine preferably a little less than definite value nonmetallic impurity element amplitudes in the sodium diuranate, on show the data fit processing requirement.
1.2 dissolving
By uranium content 67.28% in the sodium diuranate raw material, moisture content 24.56% is considered process and is analyzed loss, calculates 30 kilograms of tables of preparation 1-1 sodium diuranate nonmetallic impurity element reference material and need prepare 42 kilograms of sodium diuranate raw materials.Raw material is with dissolving in (1+1) analytical pure nitric acid, and its main reaction formula is:
Na
2U
2O
7+6HNO
3=2UO
2(NO
3)
2?+?2NaNO
3?+?3H
2O
Calculating dissolving 1 grammes per square metre uranium yellow raw material consumption (1+1) analytical pure nitric acid theoretical value according to reaction equation is 1.26mL; Actual consumption nitric acid amount need be used the nitre acidimeter with the every grammes per square metre uranium yellow of titration raw material; Its titration results is that per 1 grammes per square metre uranium yellow raw material needs (1+1) analytical pure nitric acid volume 1.2mL, and for guaranteeing to react completely, it is excessive that nitric acid needs; By excessive 15%, need with 57L (1+1) analytical pure nitric acid dissolve 42 kilopond uranium yellow raw materials altogether.Raw material dissolves at stainless steel tank, churning time 4 hours, and digestion time was greater than 24 hours.
2. filter, constant volume
2.1 filter
Material is transported to the stainless steel pressure filter through plastic pump and carries out coarse filtration after nitric acid fully dissolves, and filtrating is carried out gravity filtration through smart filter pocket again, and filter cloth is that acid and alkali-resistance is encrypted 621 types, the filtrating clarification.
2.2 constant volume
Filter back clear liquid is delivered to the scale tank constant volume through plastic pump, and about 140 liters of clear liquid volumes are settled to 160 liters with soft water, stir, and sampling analysis records solution uranium concentration 129.8 g/L, and its sulphur, phosphorus, silicon, fluorine, cl content (in the uranium base) are like following table 1-3.
Table 1-3:
| Element | S | P | Si | F | CL |
| Content mg/g (uranium) | 1.180 | 0.112 | 0.337 | 0 | 7.540 |
Solution behind the constant volume is delivered to precipitation tank in term, and scale tank is rinsed well with one-level water, and washing lotion changes precipitation tank in term in the lump over to.
3. precipitated crystal
3.1 reagent preparation
3.1.1 sodium hydroxide solution preparation
The selected reagent of preparation sodium hydroxide solution is that top grade is pure, and water is one-level water, and compound concentration is 200g/L, volume 120L.
3.1.2 mark-on liquid mix reagent preparation
The material of preparation mark-on liquid mix reagent is that top grade is pure, and water is one-level water, and its sample weighting amount calculates in the ratio of 1 kilogram of pilot scale.Preparation mark-on liquid reagent basicity is 30 g/L, volume 130L.
3.2 precipitated crystal process
With the precipitation tank in term solution stirring, heating when 52 ℃ of temperature, slowly adds sodium hydroxide solution; In the pH value is 2.4, when solution is muddy, stops to add sodium hydroxide solution; After stirring, slowly add mark-on liquid mix reagent again, at this moment phosphorus, element silicon and sodium diuranate co-precipitation; Fluorine element part and diuranate co-precipitation, when reagent all adds fashionablely, the pH value of solution value is 7.0; Behind molecular balance, continuing to add the sodium hydroxide solution adjust pH is 7.8, cooling cooling naturally; Phosphorus, silicon, fluorine content and uranium content in sampling monitoring analysis mother liquor of precipitation of ammonium, the crystal, uranium content is 64.95% in its crystal, phosphorus, silicon, fluorine content (uranium base meter) data such as following table 1-4.
Table 1-4:
| Element | P | Si | F |
| Content % | 1.02 | 1.51 | 0.187 |
4. filter, wash
4.1 filter
The deposition crystal carries out liquid-solid separation with whizzer, and centrifuge speed is used Frequency Converter Control, before filter cake does not form, opens the slow speed of revolution, prevents that thin crystalline substance from passing filter cloth, improves rotating speed then, makes liquid-solid abundant separation.
4.2 washing
Filter later crystal and contain a large amount of SODIUMNITRATE, carry out centrifuge washing with one-level water, to remove SODIUMNITRATE, reduce crystal water content as far as possible, silicon, phosphoric are difficult for being washed out, and fluorine element partly is washed out.
5. dry
The crystal that washing is the good Stainless Steel Disc of packing into is delivered to stainless steel baking oven inner drying, under 105 ℃, dries to constant weight.
6. grind, sieve, mixing
Dry good crystal grinds with grinding machine, crosses 100 order stainless steel sifts, at the abundant mixing of vortex mixer, dries to constant weight then again, weighs, and sampling analysis sulphur, phosphorus, silicon, fluorine, cl content and uranium content its data 1-5 that sees the following form.
Table 1-5:
| Element | S | P | Si | F | CL | U |
| Content % | 0.091 | 1.01 | 1.49 | 0.112 | 0.021 | 64.80 |
7. evaporation
Measure adding sodium sulfate, sodium-chlor, Sodium Fluoride add-on, fully dissolve, together add in the evaporating pan, stir the heating evaporate to dryness with the good material of mixing with one-level water.
8. grind again, sieve, mixing
Material in the evaporating pan is all taken out, grind with grinding machine once more, cross 100 order stainless steel sifts, with the abundant mixing of vortex mixer.
9. dry, analysis
The material that mixing is good is packed in the stainless dish, puts into baking oven, dries to constant weight sulphur, phosphorus, silicon, fluorine, cl content in the sampling analysis sample, its data 1-6 that sees the following form at 105 ℃.
Table 1-6:
| Element | S | P | Si | F | CL |
| Content % | 2.67 | 0.942 | 1.34 | 0.274 | 0.458 |
| RSD% | 1.4 | 1.4 | 1.6 | 3.9 | 3.1 |
See that from last table data sulphur, phosphorus, silicon, fluorine, five non-metallic elements of chlorine are all in sodium diuranate in the expection range of uncertainty of definite value value.Sample is through initial survey, bottling and uniformity testing, and the sodium diuranate sulphur that makes, phosphorus, silicon, fluorine, five nonmetallic impurity elements of chlorine reference material are qualified.
Embodiment 2
Prepare 30 kilopond uranium yellow non-metallic element reference materials, the value of definite value nonmetallic impurity element and expection uncertainty are as showing 2-1 in its sodium diuranate:
The value of definite value nonmetallic impurity element and expection uncertainty (%) in the table 2-1 sodium diuranate
| Element | S | P | Si | F | CL |
| Standard value | 0.60 | 0.15 | 0.40 | 0.10 | 0.10 |
| Combined standard uncertainty | 0.12 | 0.03 | 0.08 | 0.02 | 0.02 |
1. material dissolution
1.1 material is selected
Select sodium diuranate (barrel number 61-22) that certain ore deposit produces as raw material, its sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity constituent contents of chlorine and uranium and moisture content such as following table 2-2.
Table 2-2:
| Element (material) | S | P | Si | F | CL | U | H 2O |
| Content | 0.13% | 0.035% | 0.04% | <0.005% | 0.21% | 67.28% | 24.56% |
Require to select in the raw material sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity content of chlorine preferably a little less than definite value nonmetallic impurity element amplitudes in the sodium diuranate, on show the data fit processing requirement.
1.2 dissolving
By uranium content 67.28% in the sodium diuranate raw material, moisture content 24.56% is considered process and is analyzed loss, calculates 30 kilograms of tables of preparation 2-1 sodium diuranate nonmetallic impurity element reference material and need prepare 48 kilograms of sodium diuranate raw materials.Raw material dissolves in (1+1) analytical pure nitric acid, and its main reaction formula is:
Na
2U
2O
7+6HNO
3=2UO
2(NO
3)
2?+?2NaNO
3?+?3H
2O
Calculating dissolving 1 grammes per square metre uranium yellow raw material consumption (1+1) analytical pure nitric acid theoretical value according to reaction equation is 1.26mL; Actual consumption nitric acid amount need be used the nitre acidimeter with the every grammes per square metre uranium yellow of titration raw material; Its titration results is that per 1 grammes per square metre uranium yellow raw material needs (1+1) analytical pure nitric acid volume 1.2 mL, and for guaranteeing to react completely, it is excessive that nitric acid need be used; By excessive 15%, need with 66L (1+1) analytical pure nitric acid dissolve 48 kilopond uranium yellow raw materials altogether.Raw material dissolves at stainless steel tank, churning time 4 hours, and digestion time was greater than 24 hours.
2. filter, constant volume
2.1 filter
Material is transported to the stainless steel pressure filter through plastic pump and carries out coarse filtration after nitric acid fully dissolves, and filtrating is carried out gravity filtration through smart filter pocket again, the filtrating clarification.
2.2 constant volume
Filter back clear liquid is delivered to the scale tank constant volume through plastic pump, and about 130 liters of clear liquid volumes are settled to 160 liters with soft water, stir, and sampling analysis records solution uranium concentration 145.0 g/L, and its sulphur, phosphorus, silicon, fluorine, cl content (in the uranium base) are like following table 2-3.
Table 2-3
| Element | S | P | Si | F | CL |
| Content mg/g (uranium) | 1.301 | 0.143 | 0.319 | 0 | 6.802 |
Solution behind the constant volume is delivered to precipitation tank in term, and scale tank is rinsed well with one-level water, and washing lotion changes precipitation tank in term in the lump over to.
3. precipitated crystal
3.1 reagent preparation
3.1.1 sodium hydroxide solution preparation
The selected reagent of preparation sodium hydroxide solution is that top grade is pure, and water is one-level water, and compound concentration is 200g/L, volume 120L.
3.1.2 mark-on liquid mix reagent preparation
The material of preparation mark-on liquid mix reagent is that top grade is pure, and water is one-level water, and its sample weighting amount calculates in the ratio of 1 kilogram of pilot scale.Preparation mark-on liquid reagent basicity is 30 g/L, volume 131L.
3.2 precipitated crystal process
With the precipitation tank in term solution stirring, heating when 60 ℃ of temperature, slowly adds sodium hydroxide solution; In the pH value is 2, when solution is muddy, stops to add sodium hydroxide solution, after stirring; Slowly add mark-on liquid mix reagent again, phosphorus, element silicon and sodium diuranate co-precipitation at this moment, fluorine element part and diuranate co-precipitation are when reagent all adds fashionable; The pH value of solution value is 6.2, and behind molecular balance, continuing to add the sodium hydroxide solution adjust pH is 7.5, cooling cooling naturally; Phosphorus, silicon, fluorine content and uranium content in sampling monitoring analysis mother liquor of precipitation of ammonium, the crystal, uranium content is 71.62% in its crystal, phosphorus, silicon, fluorine content (uranium base meter) data such as following table 2-4.
Table 2-4
| Element | P | Si | F |
| Content % | 0.154 | 0.392 | 0.098 |
4. filter, wash
4.1 filter
The deposition crystal carries out liquid-solid separation with whizzer, and centrifuge speed is used Frequency Converter Control, before filter cake does not form, opens the slow speed of revolution, prevents that thin crystalline substance from passing filter cloth, improves rotating speed then, makes liquid-solid abundant separation.
4.2 washing
Filter later crystal and contain a large amount of SODIUMNITRATE, carry out centrifuge washing with one-level water, to remove SODIUMNITRATE, reduce crystal water content as far as possible, silicon, phosphoric are difficult for being washed out, and fluorine element partly is washed out.
5. dry
The crystal that washing is the good Stainless Steel Disc of packing into is delivered to stainless steel baking oven inner drying, under 108 ℃, dries to constant weight.
6. grind, sieve, mixing
Dry good crystal grinds with grinding machine, crosses 100 order stainless steel sifts, at the abundant mixing of vortex mixer, dries to constant weight then again, weighs, and sampling analysis sulphur, phosphorus, silicon, fluorine, cl content and uranium content its data 2-5 that sees the following form.
Table 2-5:
| Element | S | P | Si | F | CL | U |
| Content % | 0.072 | 0.149 | 0.390 | 0.052 | 0.018 | 71.64 |
7. evaporation
Measure adding sodium sulfate, sodium-chlor, Sodium Fluoride add-on, fully dissolve, together add in the evaporating pan, stir the heating evaporate to dryness with the good material of mixing with one-level water.
8. grind again, sieve, mixing
Material in the evaporating pan is all taken out, grind with grinding machine once more, cross 100 order stainless steel sifts, with the abundant mixing of vortex mixer.
9. dry, analysis
The material that mixing is good is packed in the stainless dish, puts into baking oven, dries to constant weight sulphur, phosphorus, silicon, fluorine, cl content in the sampling analysis sample, its data 2-6 that sees the following form at 108 ℃.
Table 2-6:
| Element | S | P | Si | F | CL |
| Content % | 0.621 | 0.138 | 0.355 | 0.105 | 0.111 |
| RSD% | 2.3 | 0.9 | 2.0 | 1.7 | 2.3 |
See that from last table data sulphur, phosphorus, silicon, fluorine, five non-metallic elements of chlorine are all in sodium diuranate in the expection range of uncertainty of definite value value.Sample is through initial survey, bottling and uniformity testing, and the sodium diuranate sulphur that makes, phosphorus, silicon, fluorine, five nonmetallic impurity elements of chlorine reference material are qualified.
Embodiment three
Prepare 4 kilopond uranium yellow non-metallic element reference materials, the value of definite value nonmetallic impurity element and expection uncertainty such as following table 3-1 in its sodium diuranate:
The value of definite value nonmetallic impurity element and expection uncertainty (%) in the table 3-1 sodium diuranate
| Element | S | P | Si | F | CL |
| Standard value | 3.0 | 1.0 | 1.5 | 0.3 | 0.5 |
| Combined standard uncertainty | 0.6 | 0.2 | 0.3 | 0.06 | 0.1 |
1. material dissolution
1.1 material is selected
Select sodium diuranate (barrel number 61-22) that certain ore deposit produces as raw material, its sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity constituent contents of chlorine and uranium and moisture content such as following table 3-2.
Table 3-2:
| Element (material) | S | P | Si | F | CL | U | H 2O |
| Content | 0.13% | 0.035% | 0.04% | <0.005% | 0.21% | 67.28% | 24.56% |
Require to select in the raw material sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity content of chlorine preferably a little less than definite value nonmetallic impurity element amplitudes in the sodium diuranate, on show the data fit processing requirement.
1.2 dissolving
By uranium content 67.28% in the sodium diuranate raw material, moisture content 24.56% is considered process and is analyzed loss, calculates 4 kilograms of tables of preparation 3-1 sodium diuranate nonmetallic impurity element reference material and need prepare 5.6 kilograms of sodium diuranate raw materials.Raw material is with dissolving in (1+1) analytical pure nitric acid, and its main reaction formula is:
Na
2U
2O
7+6HNO
3=2UO
2(NO
3)
2?+?2NaNO
3?+?3H
2O
Calculating dissolving 1 grammes per square metre uranium yellow raw material consumption (1+1) analytical pure nitric acid theoretical value according to reaction equation is 1.26mL; Actual consumption nitric acid amount need be used the nitre acidimeter with the every grammes per square metre uranium yellow of titration raw material; Its titration results is that per 1 grammes per square metre uranium yellow raw material needs (1+1) analytical pure nitric acid volume 1.2mL, and for guaranteeing to react completely, it is excessive that nitric acid needs; By excessive 15%, need with 7.7L (1+1) analytical pure nitric acid dissolve 5.6 kilopond uranium yellow raw materials altogether.Raw material dissolves at stainless steel tank, churning time 4 hours, and digestion time was greater than 24 hours.
2. filter, constant volume
2.1 filter
Material is transported to the stainless steel pressure filter through plastic pump and carries out coarse filtration after nitric acid fully dissolves, and filtrating is carried out gravity filtration through smart filter pocket again, and filter cloth is that acid and alkali-resistance is encrypted 621 types, the filtrating clarification.
2.2 constant volume
Filter back clear liquid is settled to 22 liters with soft water, stirs, and sampling analysis records solution uranium concentration 126.5g/L, and its sulphur, phosphorus, silicon, fluorine, cl content (in the uranium base) are like following table 3-3.
Table 3-3
| Element | S | P | Si | F | CL |
| Content mg/g (uranium) | 1.230 | 0.102 | 0.352 | 0 | 7.126 |
Solution behind the constant volume is delivered to precipitation tank in term, and scale tank is rinsed well with one-level water, and washing lotion changes precipitation tank in term in the lump over to.
3. precipitated crystal
3.1 reagent preparation
3.1.1 sodium hydroxide solution preparation
The selected reagent of preparation sodium hydroxide solution is that top grade is pure, and water is one-level water, and compound concentration is 200g/L, volume 15L.
3.1.2 mark-on liquid mix reagent preparation
The material of preparation mark-on liquid mix reagent is that top grade is pure, and water is one-level water, and its sample weighting amount calculates in the ratio of 1 kilogram of pilot scale.Preparation mark-on liquid reagent basicity is 30 g/L, volume 17L.
3.2 precipitated crystal process
With the precipitation tank in term solution stirring, heating when 40 ℃ of temperature, slowly adds sodium hydroxide solution; In the pH value is 2.1, when solution is muddy, stops to add sodium hydroxide solution; After stirring, slowly add mark-on liquid mix reagent again, at this moment phosphorus, element silicon and sodium diuranate co-precipitation; Fluorine element part and diuranate co-precipitation, when reagent all adds fashionablely, the pH value of solution value is 6.0; Behind molecular balance, continuing to add the sodium hydroxide solution adjust pH is 7.3, cooling cooling naturally; Phosphorus, silicon, fluorine content and uranium content in sampling monitoring analysis mother liquor of precipitation of ammonium, the crystal, uranium content is 64.20% in its crystal, phosphorus, silicon, fluorine content (uranium base meter) data such as following table 3-4.
Table 3-4:
| Element | P | Si | F |
| Content % | 1.13 | 1.58 | 0.208 |
4. filter, wash
4.1 filter
The deposition crystal carries out liquid-solid separation with whizzer, and centrifuge speed is used Frequency Converter Control, before filter cake does not form, opens the slow speed of revolution, prevents that thin crystalline substance from passing filter cloth, improves rotating speed then, makes liquid-solid abundant separation.
4.2 washing
Filter later crystal and contain a large amount of SODIUMNITRATE, carry out centrifuge washing with one-level water, to remove SODIUMNITRATE, reduce crystal water content as far as possible, silicon, phosphoric are difficult for being washed out, and fluorine element partly is washed out.
5. dry
The crystal that washing is the good Stainless Steel Disc of packing into is delivered to stainless steel baking oven inner drying, under 110 ℃, dries to constant weight.
6. grind, sieve, mixing
Dry good crystal grinds with grinding machine, crosses 100 order stainless steel sifts, at the abundant mixing of vortex mixer, dries to constant weight then again, weighs, and sampling analysis sulphur, phosphorus, silicon, fluorine, cl content and uranium content its data 3-5 that sees the following form.
Table 3-5:
| Element | S | P | Si | F | CL | U |
| Content % | 0.101 | 1.10 | 1.58 | 0.132 | 0.061 | 64.77 |
7. evaporation
Measure adding sodium sulfate, sodium-chlor, Sodium Fluoride add-on, fully dissolve, together add in the evaporating pan, stir the heating evaporate to dryness with the good material of mixing with one-level water.
8. grind again, sieve, mixing
Material in the evaporating pan is all taken out, grind with grinding machine once more, cross 100 order stainless steel sifts, with the abundant mixing of vortex mixer.
9. dry, analysis
The material that mixing is good is packed in the stainless dish, puts into baking oven, dry to constant weight at 110 ℃, and sulphur, phosphorus, silicon, fluorine, cl content in the sampling analysis sample, its data 3-6 that sees the following form:
Table 3-6
| Element | S | P | Si | F | CL |
| Content % | 2.81 | 0.922 | 1.44 | 0.283 | 0.456 |
| RSD% | 1.3 | 1.7 | 1.5 | 3.6 | 3.5 |
See that from last table data sulphur, phosphorus, silicon, fluorine, five non-metallic elements of chlorine are all in sodium diuranate in the expection range of uncertainty of definite value value.Sample is through initial survey, bottling and uniformity testing, and the sodium diuranate sulphur that makes, phosphorus, silicon, fluorine, five nonmetallic impurity elements of chlorine reference material are qualified.
Embodiment 4
Prepare 4 kilopond uranium yellow non-metallic element reference materials, the value of definite value nonmetallic impurity element and expection uncertainty such as following table 4-1 in its sodium diuranate:
The value of definite value nonmetallic impurity element and expection uncertainty (%) in the table 4-1 sodium diuranate
| Element | S | P | Si | F | CL |
| Standard value | 3.0 | 1.0 | 1.5 | 0.3 | 0.5 |
| Combined standard uncertainty | 0.6 | 0.2 | 0.3 | 0.06 | 0.1 |
1. material dissolution
1.1 material is selected
Select sodium diuranate (barrel number 147) that certain ore deposit produces as raw material, its sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity constituent contents of chlorine and uranium and moisture content such as following table 4-2:
Table 4-2
| Element (material) | S | P | Si | F | CL | U | H 2O |
| Content | 0.75% | 0.006% | 0.13% | 0.1% | 0.13% | 65.98% | 26.82% |
Require to select in the raw material sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity content of chlorine preferably a little less than definite value nonmetallic impurity element amplitudes in the sodium diuranate, on show the data fit processing requirement.
1.2 dissolving
By uranium content 65.98% in the sodium diuranate raw material, moisture content 26.82% is considered process and is analyzed loss, calculates 4 kilograms of tables of preparation 4-1 sodium diuranate nonmetallic impurity element reference material and need prepare 5.8 kilograms of sodium diuranate raw materials.Raw material is with dissolving in (1+1) analytical pure nitric acid, and its main reaction formula is:
Na
2U
2O
7+6HNO
3=2UO
2(NO
3)
2?+?2NaNO
3?+?3H
2O
Calculating dissolving 1 grammes per square metre uranium yellow raw material consumption (1+1) analytical pure nitric acid theoretical value according to reaction equation is 1.26mL; Actual consumption nitric acid amount need be used the nitre acidimeter with the every grammes per square metre uranium yellow of titration raw material; Its titration results is that per 1 grammes per square metre uranium yellow raw material needs (1+1) analytical pure nitric acid volume 1.18mL, and for guaranteeing to react completely, it is excessive that nitric acid needs; By excessive 15%, need with 7.9 L (1+1) analytical pure nitric acid dissolve, 5.8 kilopond uranium yellow raw materials altogether.Raw material dissolves at stainless steel tank, churning time 4 hours, and digestion time was greater than 24 hours.
2. filter, constant volume
2.1 filter
Material carries out gravity filtration after nitric acid fully dissolves, obtain filtering the back clear liquid.
2.2 constant volume
Filter back clear liquid is settled to 22 liters with soft water, stirs, and sampling analysis records solution uranium concentration 121.3 g/L, and its sulphur, phosphorus, silicon, fluorine, cl content (in the uranium base) are like following table 4-3:
Table 4-3
| Element | S | P | Si | F | CL |
| Content mg/g (uranium) | 6.282 | 0.181 | 0.931 | 0.799 | 4.627 |
Solution behind the constant volume is delivered to precipitation tank in term, and scale tank is rinsed well with one-level water, and washing lotion changes precipitation tank in term in the lump over to.
3. precipitated crystal
3.1 reagent preparation
3.1.1 sodium hydroxide solution preparation
The selected reagent of preparation sodium hydroxide solution is that top grade is pure, and water is one-level water, and compound concentration is 200g/L, volume 15L.
3.1.2 mark-on liquid mix reagent preparation
The material of preparation mark-on liquid mix reagent is that top grade is pure, and water is one-level water, and its sample weighting amount calculates in the ratio of 1 kilogram of pilot scale.Preparation mark-on liquid reagent basicity is 30 g/L, volume 17L.
3.2 precipitated crystal process
With the precipitation tank in term solution stirring, heating when 60 ℃ of temperature, slowly adds sodium hydroxide solution; In the pH value is 3, when solution is muddy, stops to add sodium hydroxide solution, after stirring; Slowly add mark-on liquid mix reagent again, phosphorus, element silicon and sodium diuranate co-precipitation at this moment, fluorine element part and diuranate co-precipitation are when reagent all adds fashionable; The pH value of solution value is 6.8, and behind molecular balance, continuing to add the sodium hydroxide solution adjust pH is 7.5, cooling cooling naturally; Phosphorus, silicon, fluorine content and uranium content in sampling monitoring analysis mother liquor of precipitation of ammonium, the crystal, uranium content is 65.22% in its crystal, phosphorus, silicon, fluorine content (uranium base meter) data such as following table 4-4:
Table 4-4
| Element | P | Si | F |
| Content % | 1.09 | 1.62 | 0.195 |
4. filter, wash
4.1 filter
The deposition crystal carries out liquid-solid separation with whizzer, and centrifuge speed is used Frequency Converter Control, before filter cake does not form, opens the slow speed of revolution, prevents that thin crystalline substance from passing filter cloth, improves rotating speed then, makes liquid-solid abundant separation.
4.2 washing
Filter later crystal and contain a large amount of SODIUMNITRATE, carry out centrifuge washing with one-level water, to remove SODIUMNITRATE, reduce crystal water content as far as possible, silicon, phosphoric are difficult for being washed out, and fluorine element partly is washed out.
5. dry
The crystal that washing is the good Stainless Steel Disc of packing into is delivered to stainless steel baking oven inner drying, under 110 ℃, dries to constant weight.
6. grind, sieve, mixing
The crystal that drying is good grinds with grinding machine, crosses 100 order stainless steel sifts, at the abundant mixing of vortex mixer, dries to constant weight then again, weighs, and sampling analysis sulphur, phosphorus, silicon, fluorine, cl content and uranium content its data 4-5 that sees the following form:
Table 4-5
| Element | S | P | Si | F | CL | U |
| Content % | 0.128 | 0.111 | 1.59 | 0.122 | 0.045 | 65.82 |
7. evaporation
Measure adding sodium sulfate, sodium-chlor, Sodium Fluoride add-on, fully dissolve, together add in the evaporating pan, stir the heating evaporate to dryness with the good material of mixing with one-level water.
8. grind again, sieve, mixing
Material in the evaporating pan is all taken out, grind with grinding machine once more, cross 100 order stainless steel sifts, with the abundant mixing of vortex mixer.
9. dry, analysis
The material that mixing is good is packed in the stainless dish, puts into baking oven, dry to constant weight at 110 ℃, and sulphur, phosphorus, silicon, fluorine, cl content in the sampling analysis sample, its data 4-6 that sees the following form:
Table 4-6
| Element | S | P | Si | F | CL |
| Content % | 2.72 | 0.91 | 1.39 | 0.281 | 0.467 |
| RSD% | 1.7 | 1.4 | 1.5 | 2.1 | 2.2 |
See that from last table data sulphur, phosphorus, silicon, fluorine, five non-metallic elements of chlorine are all in sodium diuranate in the expection range of uncertainty of definite value value.Sample is through initial survey, bottling and uniformity testing, and the sodium diuranate sulphur that makes, phosphorus, silicon, fluorine, five nonmetallic impurity elements of chlorine reference material are qualified.
Embodiment five
Prepare 4 kilopond uranium yellow non-metallic element reference materials, the value of definite value nonmetallic impurity element and expection uncertainty such as following table 5-1 in its sodium diuranate:
The value of definite value nonmetallic impurity element and expection uncertainty (%) in the table 5-1 sodium diuranate
| Element | S | P | Si | F | CL |
| Standard value | 0.60 | 0.15 | 0.40 | 0.10 | 0.10 |
| Combined standard uncertainty | 0.12 | 0.03 | 0.08 | 0.02 | 0.02 |
1. material dissolution
1.1 material is selected
Select sodium diuranate (barrel number 147) that certain ore deposit produces as raw material, its sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity constituent contents of chlorine and uranium and moisture content such as following table 5-2:
Table 5-2
| Element (material) | S | P | Si | F | CL | U | H 2O |
| Content | 0.75% | 0.006% | 0.13% | 0.1% | 0.13% | 65.98% | 26.82% |
Sulphur, chlorine foreign matter content are higher than definite value sulphur in the sodium diuranate, chlorine element amplitudes in the last table data; Because fluorine, chlorine, sulphur trigram element can wash in washing process down; Content requirement can suitably be relaxed, if solvable phosphorus, sila matter content are higher than the value in the definite value in the raw material, can carry out chemical treatment; Can adopt elder generation with carrying out measures such as IX or refining uranyl nitrate behind the material dissolution again, reduce its content and get final product.Preferably select sulphur in the raw material, phosphorus, silicon, fluorine, five nonmetallic impurity content of chlorine a little less than definite value nonmetallic impurity element amplitudes in the sodium diuranate.
1.2 dissolving
By uranium content 65.98% in the sodium diuranate raw material, moisture content 26.82% is considered process and is analyzed loss, calculates 4 kilograms of tables of preparation 5-1 sodium diuranate nonmetallic impurity element reference material and need prepare 6 kilograms of sodium diuranate raw materials.Raw material is with dissolving in (1+1) analytical pure nitric acid, and its main reaction formula is:
Na
2U
2O
7+6HNO
3=2UO
2(NO
3)
2?+?2NaNO
3?+?3H
2O
Calculating dissolving 1 grammes per square metre uranium yellow raw material consumption (1+1) analytical pure nitric acid theoretical value according to reaction equation is 1.26mL; Actual consumption nitric acid amount need be used the nitre acidimeter with the every grammes per square metre uranium yellow of titration raw material; Its titration results is that per 1 grammes per square metre uranium yellow raw material needs (1+1) analytical pure nitric acid volume 1.18mL, and for guaranteeing to react completely, it is excessive that nitric acid needs; By excessive 15%, need with 8.1 L (1+1) analytical pure nitric acid dissolve, 6 kilopond uranium yellow raw materials altogether.Raw material dissolves at stainless steel tank, churning time 4 hours, and digestion time was greater than 24 hours.
2. filter, constant volume
2.1 filter
Material carries out gravity filtration after nitric acid fully dissolves, obtain filtering the back clear liquid.
2.2 constant volume
Filter back clear liquid is settled to 22 liters with soft water, stirs, and sampling analysis records solution uranium concentration 131.8 g/L, and its sulphur, phosphorus, silicon, fluorine, cl content (in the uranium base) are like following table 5-3:
Table 5-3
| Element | S | P | Si | F | CL |
| Content mg/g (uranium) | 6.009 | 0.169 | 1.062 | 0.762 | 4.303 |
Solution behind the constant volume is delivered to precipitation tank in term, and scale tank is rinsed well with one-level water, and washing lotion changes precipitation tank in term in the lump over to.
3. precipitated crystal
3.1 reagent preparation
3.1.1 sodium hydroxide solution preparation
The selected reagent of preparation sodium hydroxide solution is that top grade is pure, and water is one-level water, and compound concentration is 200g/L, volume 15L.
3.1.2 mark-on liquid mix reagent preparation
The material of preparation mark-on liquid mix reagent is that top grade is pure, and water is one-level water, and its sample weighting amount calculates in the ratio of 1 kilogram of pilot scale.Preparation mark-on liquid reagent basicity is 30 g/L, volume 17L.
3.2 precipitated crystal process
With the precipitation tank in term solution stirring, heating when 58 ℃ of temperature, slowly adds sodium hydroxide solution; In the pH value is 2.3, when solution is muddy, stops to add sodium hydroxide solution; After stirring, slowly add mark-on liquid mix reagent again, at this moment phosphorus, element silicon and sodium diuranate co-precipitation; Fluorine element part and diuranate co-precipitation, when reagent all adds fashionablely, the pH value of solution value is 6.2; Behind molecular balance, continuing to add the sodium hydroxide solution adjust pH is 7.1, cooling cooling naturally; Phosphorus, silicon, fluorine content and uranium content in sampling monitoring analysis mother liquor of precipitation of ammonium, the crystal, uranium content is 69.15% in its crystal, phosphorus, silicon, fluorine content (uranium base meter) data such as following table 5-4:
Table 5-4
| Element | P | Si | F |
| Content % | 0.162 | 0.412 | 0.086 |
4. filter, wash
4.1 filter
The deposition crystal carries out liquid-solid separation with whizzer, and centrifuge speed is used Frequency Converter Control, before filter cake does not form, opens the slow speed of revolution, prevents that thin crystalline substance from passing filter cloth, improves rotating speed then, makes liquid-solid abundant separation.
4.2 washing
Filter later crystal and contain a large amount of SODIUMNITRATE, carry out centrifuge washing with one-level water, to remove SODIUMNITRATE, reduce crystal water content as far as possible, silicon, phosphoric are difficult for being washed out, and fluorine element partly is washed out.
5. dry
The crystal that washing is the good Stainless Steel Disc of packing into is delivered to stainless steel baking oven inner drying, under 105 ℃, dries to constant weight.
6. grind, sieve, mixing
The crystal that drying is good grinds with grinding machine, crosses 100 order stainless steel sifts, at the abundant mixing of vortex mixer, dries to constant weight then again, weighs, and sampling analysis sulphur, phosphorus, silicon, fluorine, cl content and uranium content its data 5-5 that sees the following form:
Table 5-5
| Element | S | P | Si | F | CL | U |
| Content % | 0.066 | 0.159 | 0.410 | 0.063 | 0.032 | 68.21 |
7. evaporation
Measure adding sodium sulfate, sodium-chlor, Sodium Fluoride add-on, fully dissolve, together add in the evaporating pan, stir the heating evaporate to dryness with the good material of mixing with one-level water.
8. grind again, sieve, mixing
Material in the evaporating pan is all taken out, grind with grinding machine once more, cross 100 order stainless steel sifts, with the abundant mixing of vortex mixer.
9. dry, analysis
The material that mixing is good is packed in the stainless dish, puts into baking oven, dry to constant weight at 105 ℃, and sulphur, phosphorus, silicon, fluorine, cl content in the sampling analysis sample, its data 5-6 that sees the following form:
Table 5-6
| Element | S | P | Si | F | CL |
| Content % | 0.592 | 0.146 | 0.399 | 0.091 | 0.894 |
| RSD% | 2.0 | 1.2 | 1.8 | 1.9 | 2.5 |
See that from last table data sulphur, phosphorus, silicon, fluorine, five non-metallic elements of chlorine are all in sodium diuranate in the expection range of uncertainty of definite value value.Sample is through initial survey, bottling and uniformity testing, and the sodium diuranate sulphur that makes, phosphorus, silicon, fluorine, five nonmetallic impurity elements of chlorine reference material are qualified.
The reference material of the present invention's preparation is used for the quality control of uranium compound fluorine, chlorine, sulphur, phosphorus, silica test, the calibration analyte instrument, and the accuracy and the safety of evaluation and check analysis method can be made transmission of quantity value.The dry cleansing place is deposited in the sealing of this reference material, needs under 105 ℃～110 ℃ temperature condition, to be dried to constant weight before using.
Claims (1)
1. a diuranate non-metallic element reference material preparation technology is characterized in that comprising the steps:
(1). with the sodium diuranate is raw material, and sulphur, phosphorus, silicon, fluorine, five nonmetallic impurity content of chlorine will be lower than definite value nonmetallic impurity element amplitudes in the sodium diuranate in this raw material;
(2). fully dissolve said raw material with analytical pure nitric acid, obtain lysate;
(3). the lysate that step (2) is obtained filters, and carries out liquid-solid separation, and the clear liquid constant volume that obtains after the separation is measured sulphur, phosphorus, silicon, fluorine, five non-metallic element content of chlorine and uranium content;
(4). the clear liquid behind the constant volume changes precipitation tank in term over to; Stir; Heating; When 40 ℃～60 ℃ of temperature; Regulate acidity with sodium hydroxide solution; When the pH value is 2～3 solution commentaries on classics muddiness; Stop to add sodium hydroxide solution; After waiting to stir, in solution, add reagent, this reagent is to contain phosphorus; Silicon; The NaOH mark-on liquid mix reagent of fluorine element; With the phosphorus that is difficult for being got off by water washing; Silicon binomial element and sodium diuranate co-precipitation; Fluorine part and sodium diuranate co-precipitation, add whole reagent after, control acidity is 6.0～7.0 in the pH value; Behind the molecular balance; Continuing to add sodium hydroxide solution to acidity is 7.1～7.8 in the pH value, cooling cooling naturally, phosphorus in sampling monitoring analysis mother liquor of precipitation of ammonium and the crystal; Silicon; Whether fluorine content and uranium content reach;
(5). cooled mother liquor of precipitation of ammonium of step (4) and crystal are used centrifugal filter centrifuging; Crystal is with after mother liquor of precipitation of ammonium is separated; Crystal with one-level water centrifuge washing, is removed wherein SODIUMNITRATE in whizzer, wherein the part fluorine element also washs from crystal;
(6). the sodium diuranate crystal after will washing is transferred to the baking oven inner drying, under 105 ℃～110 ℃, dries to constant weight;
(7). the sodium diuranate crystal that will be dried to constant weight grinds, and crosses 100 order stainless steel sifts, sends into abundant mixing in the vortex mixer then, is dried to constant weight again and also accurately weighs, and analyzes sulphur, phosphorus, silicon, fluorine, cl content and uranium content;
(8). accurate weighing sulphur, fluorine, the plain add-on of chlorine trigram; Be prepared into solution; Stir in evaporating pan with the crystal powder after grinding; Heating evaporation is blended into sulphur, phosphorus, chlorine trigram element in the diuranate through the slurrying method of evaporation, is evaporated to the dry doubling taking-up and in 105 ℃～110 ℃ baking ovens, dries to constant weight;
(9). with the sodium diuranate crystal regrinding that step (8) dries to constant weight, cross 100 order stainless steel sifts, send into abundant mixing in the vortex mixer;
(10). the good sodium diuranate crystal of step (9) mixing is put into 105 ℃～110 ℃ drying in oven to constant weights obtain sample; Sample is through the homogeneity initial survey; The bottling and carry out uniformity testing qualified after, promptly make diuranate sulphur, phosphorus, silicon, fluorine, five non-metallic element reference materials of chlorine.
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| CN109443874A (en) * | 2018-11-22 | 2019-03-08 | 核工业北京化工冶金研究院 | Uranium and impurity element standard substance preparation method in a kind of triuranium octoxide |
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| CN114368786A (en) * | 2021-12-03 | 2022-04-19 | 中核沽源铀业有限责任公司 | Sodium diuranate impurity content reduction method based on washing before filtration |
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Application publication date: 20120502 |