CN108267474A - The assay method of nitrogen content in a kind of MOX pellets - Google Patents
The assay method of nitrogen content in a kind of MOX pellets Download PDFInfo
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- CN108267474A CN108267474A CN201711446107.9A CN201711446107A CN108267474A CN 108267474 A CN108267474 A CN 108267474A CN 201711446107 A CN201711446107 A CN 201711446107A CN 108267474 A CN108267474 A CN 108267474A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The present invention relates to fuel pellet detection fields, specifically disclose a kind of assay method of nitrogen content in MOX pellets, include the following steps：Step 1：Sample preparation；Step 2：Instrument prepares；Step 3：Blank correction；Step 4：Standard specimen corrects；Step 5：Sample measures.The method of the present invention can realize quick, the Accurate Determining of nitrogen impurity content in MOX pellets, and under the conditions of sample size is 0.050g, the detection of nitrogen impurity content is limited to 4.8 μ g/g；In the case where nitrogen content is the level of 60 μ g/g, precision of measurement is better than 5%.
Description
Technical field
The invention belongs to fuel pellet detection fields, and in particular to the assay method of nitrogen content in a kind of MOX pellets.
Background technology
China's Experiment Fast Reactor mixed oxidization uranium plutonium fuel (MOX) core nitrogen impurity content in the block is to the various physical of pellet
Can have larger impact, be that pellet manufactures the impurity element that must be monitored in each link, at the same be also MOX pellets whether qualified skill
One of art index.
The method standard ASTM C698-2010 of the nitrogen content in mixed oxidization uranium plutonium material are measured at present《Core grade mixes oxygen
Change uranium plutonium ((U, Pu) O2) chemistry, mass spectrum and the standard test method of spectrochemical analysis》In, it is to be steamed using Nessler's reagent
It evaporates spectrophotometry and carries out nitrogen analysis, this method needs to dissolve sample, nitrogen distillation separation, Nessler's reagent are shown
Color, apparatus measures, Specification Curve of Increasing and calculating and etc., for 3 μ g nitrogen, the relative standard deviation of unitary determination is
20%, it is seen that the analysis method long flow path, trivial operations, precision of measurement be not also high.
At present, conjunction is widely used in using inert gas high-temperature fusion-thermal conductivity method as the blood urea/nitrogen analyzer of measuring principle on the market
The measure of nitrogen in the materials such as gold, ceramics, metal and its oxide, and with high degree of automation, high sensitivity, accuracy it is high and
The features such as analyze speed is fast.But the particularity of radioactive material detection is limited to, is surveyed using inert gas high-temperature fusion-thermal conductivity method
The technology of nitrogen content in MOX pellets is determined there is not yet publication and open report.
Invention content
The purpose of the present invention is to provide a kind of assay methods of nitrogen content in MOX pellets, can accurately and rapidly measure
Nitrogen impurity content in MOX pellets.
Technical scheme is as follows：
The assay method of nitrogen content, includes the following steps in a kind of MOX pellets：
Step 1：Sample preparation
After MOX pellets sample progress physics is crushed, 0.050g~0.100g samples are weighed；
Step 2：Instrument prepares
1) before use, be switched on pre- more than thermal nitrogen analyzer 30min, and gas leakage detection, gas leakage detection are carried out after instrument stabilizer
By rear, acquiescence input sample quality is 1.000g, and n times skip test is carried out respectively using N number of empty graphite crucible, 3≤N≤5,
Ensure that the nitrogen content mass percent of blank is respectively less than and be equal to 0.0005%, blank is without exception, and instrument is made to keep moderately good
Working condition；
2) setting blood urea/nitrogen analyzer analyzes power between 4900~5500W, and degassing power takes off between 5800~6200W
Gas number is 2~3 times, and for degassing time between 30~50s, comparison level is 0.1~5.0%；
Step 3：Blank correction
M graphite crucible is respectively put into the nickel basket that the M specification of quality is 1g and carries out skip test, 3≤M≤5, acquiescence
Input sample quality is 1.000g, and the nitrogen content mass percent for choosing blank is less than or equal to 0.001% three effective blank
Value carries out blank correction；
Step 4：Standard specimen corrects
The accurate quality for weighing 3~5 standard steel samples, mass value are accurate to 0.001g, are respectively charged into nickel basket, input mark
It is measured after the quality of quasi- steel sample, using the measured value in the nitrogen content standard value range of standard steel sample as virtual value,
Three virtual values are chosen in analysis software to be corrected；
Step 5：Sample measures
Nickel basket equipped with sample is put into the measurement that nitrogen impurity content in sample is completed in blood urea/nitrogen analyzer, blood urea/nitrogen analyzer is automatic
Measurement result is calculated and be shown.
The graphite crucible is set crucible.
In step 5, after replacing the interior crucible in set crucible, set crucible is put under blood urea/nitrogen analyzer electrode furnace on electrode, so
Nickel basket equipped with sample is put into the falling in sample sliding block of blood urea/nitrogen analyzer by input sample quality afterwards；
Perform analysis program in analysis software, blood urea/nitrogen analyzer is de-gassed set crucible in sample after processing automatically falls into
In crucible, the measurement of nitrogen impurity content in sample is completed, measurement result is calculated and be shown in blood urea/nitrogen analyzer automatically.
When to carrying out parallel determination with a batch of sample and single sample, step 2~step 4 does not repeat.
Step 4 estimates the nitrogen content in sample before standard steel sample is weighed, and the nitrogen content of the standard steel sample of selection should approach
In the nitrogen quantity of tested sample, to improve the accuracy of measurement result.
In step 1, MOX pellet samples are put into progress physics in agate mortar and are crushed.
In step 1, sample fragment is added in the nickel basket weighed, weighs the nickel basket gross mass equipped with sample, sample matter
Amount is equal to the nickel basket gross mass equipped with sample and subtracts nickel basket quality.
It in step 2, sets blood urea/nitrogen analyzer and analyzes power as 5000W, degassing power is 6000W, and degassing number is 2 times, is taken off
The gas time be 35s, comparison level 1.0%.
Under the conditions of sample size is 0.050g, the detection of this method is limited to 4.8 μ g/g；In the level that nitrogen content is 60 μ g/g
Under, precision is better than 5%.
The blood urea/nitrogen analyzer is using inert gas high-temperature fusion-thermal conductivity method as measuring principle.
The remarkable result of the present invention is：
The method of the present invention can realize quick, the Accurate Determining of nitrogen impurity content in MOX pellets, be 0.050g in sample size
Under the conditions of, the detection of nitrogen impurity content is limited to 4.8 μ g/g；In the case where nitrogen content is the level of 60 μ g/g, precision of measurement is better than
5%.
Description of the drawings
Fig. 1 is the assay method flow chart of nitrogen content in MOX pellets.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail the present invention.
The assay method of nitrogen content, includes the following steps in a kind of MOX pellets：
Step 1：Sample preparation
MOX pellet samples are put into agate mortar and carry out after physics crushes, weighing 0.050g~0.100g samples, specifically
Method is：Sample fragment is added in the nickel basket weighed, sample size is made to weigh the nickel equipped with sample for 0.050g~0.100g
Basket gross mass, sample quality are equal to the nickel basket gross mass equipped with sample and subtract nickel basket quality；
Step 2：Instrument prepares
1) before use, be switched on pre- more than thermal nitrogen analyzer 30min, and gas leakage detection, gas leakage detection are carried out after instrument stabilizer
By rear, acquiescence input sample quality is 1.000g, and n times skip test is carried out respectively using N number of empty graphite crucible, 3≤N≤5,
Ensure that the nitrogen content mass percent of blank is respectively less than and be equal to 0.0005%, blank is without exception, and instrument is made to keep moderately good
Working condition；The graphite crucible is set crucible；
2) setting blood urea/nitrogen analyzer analyzes power between 4900~5500W, and degassing power takes off between 5800~6200W
Gas number is 2~3 times, and for degassing time between 30~50s, comparison level is 0.1~5.0%.
Step 3：Blank correction
M graphite crucible is respectively put into the nickel basket that the M specification of quality is 1g and carries out skip test, 3≤M≤5, acquiescence
Input sample quality is 1.000g, and the nitrogen content mass percent for choosing blank is less than or equal to 0.001% three effective blank
Value carries out blank correction.
Step 4：Standard specimen corrects
The accurate quality for weighing 3~5 standard steel samples, mass value are accurate to 0.001g, are respectively charged into nickel basket, input mark
It is measured after the quality of quasi- steel sample, using the measured value in the nitrogen content standard value range of standard steel sample as virtual value,
Three virtual values are chosen in analysis software to be corrected.
Before standard steel sample is weighed, the nitrogen content in sample is estimated, the nitrogen content of the standard steel sample of selection should be close to quilt
The nitrogen quantity of test specimens, to improve the accuracy of measurement result.
Step 5：Sample measures
After replacing the interior crucible in set crucible, set crucible is put under blood urea/nitrogen analyzer electrode furnace on electrode, then inputs sample
Nickel basket equipped with sample is put into the falling in sample sliding block of blood urea/nitrogen analyzer by quality；
Perform analysis program in analysis software, blood urea/nitrogen analyzer is de-gassed set crucible in sample after processing automatically falls into
In crucible, the measurement of nitrogen impurity content in sample is completed, measurement result is calculated and be shown in blood urea/nitrogen analyzer automatically.
When to carrying out parallel determination with a batch of sample and single sample, step 2~step 4 does not repeat.
Instrument its measuring principle that the method for the present invention uses be based on sample to be tested in electrode furnace high temperature under inert atmosphere
Burning, the N of generation2It is measured with thermal conductivity method, on the market using inert gas high-temperature fusion-thermal conductivity method as the nitrogen point of measuring principle
Analyzer may be applicable to the present invention.
Embodiment one
Step 1：Instrument prepares
1) before use, be switched on pre- more than thermal nitrogen analyzer 30min, and gas leakage detection, gas leakage detection are carried out after instrument stabilizer
By rear, acquiescence input sample quality is 1.000g, and n times skip test is carried out respectively using N number of empty graphite crucible, 3≤N≤5,
Ensure that the nitrogen content mass percent of blank is respectively less than and be equal to 0.0005%, blank is without exception, and instrument is made to keep moderately good
Working condition；The graphite crucible is set crucible；
2) it sets blood urea/nitrogen analyzer and analyzes power as 5000W, degassing power is 6000W, and degassing number is 2 times, degassing time
For 35s, comparison level 1.0%.
Step 2：Blank correction
4 graphite crucibles are respectively put into the nickel basket that 4 specifications of quality are 1g and carry out skip test, give tacit consent to input sample
Quality is 1.000g, chooses three effective blank values of the content mass percent of blank less than or equal to 0.001% into line blank
Correction.
Step 3：Standard specimen corrects
The accurate quality for weighing 3~5 standard steel samples, mass value are accurate to 0.001g, are respectively charged into nickel basket, input mark
It is measured after the quality of quasi- steel sample, using the measured value in the nitrogen content standard value range of standard steel sample as virtual value,
Three virtual values are chosen in analysis software to be corrected；
Nitrogen content is 79 ± 4 μ g/g in the standard steel sample selected.
Step 4：Sample measures
Set crucible is put under blood urea/nitrogen analyzer electrode furnace on electrode with crucible tongs, is measured using nickel basket as sample, weight
12 nickel baskets of repetition measurement amount.Under the conditions of sample size is 0.050g, measurement result is as follows：
Detection is limited to 3 times of standard deviation, can determine that the detection of the method for the present invention is limited to 3 times of standard deviations by embodiment one
Difference, i.e. 4.8 μ g/g.
Embodiment two
Step 1：Sample preparation；
MOX pellet samples are put into agate mortar and carry out after physics crushes, weighing 0.050g samples；
Step 2：Instrument prepares
1) before use, be switched on pre- more than thermal nitrogen analyzer 30min, and gas leakage detection, gas leakage detection are carried out after instrument stabilizer
By rear, acquiescence input sample quality is 1.000g, and n times skip test is carried out respectively using N number of empty graphite crucible, 3≤N≤5,
Ensure that the content mass percent of blank is respectively less than and be equal to 0.0005%, blank is without exception, and instrument is made to keep moderately good work
Make state；The graphite crucible is set crucible；
2) it sets blood urea/nitrogen analyzer and analyzes power as 5000W, degassing power is 6000W, and degassing number is 2 times, degassing time
For 35s, comparison level 1.0%.
Step 3：Blank correction
4 graphite crucibles are respectively put into the nickel basket that 4 specifications of quality are 1g and carry out skip test, give tacit consent to input sample
Quality is 1.000g, chooses three effective blank values of the content mass percent of blank less than or equal to 0.001% into line blank
Correction.
Step 4：Standard specimen corrects
The accurate quality for weighing 3~5 standard steel samples, mass value are accurate to 0.001g, are respectively charged into nickel basket, input mark
It is measured after the quality of quasi- steel sample, using the measured value in the nitrogen content standard value range of standard steel sample as virtual value,
Three virtual values are chosen in analysis software to be corrected；
Nitrogen content is 79 ± 4 μ g/g in the standard steel sample selected.
Step 5：Sample measures
After replacing the interior crucible in set crucible, set crucible is put under blood urea/nitrogen analyzer electrode furnace on electrode, so with crucible tongs
Nickel basket equipped with sample is put into the falling in sample sliding block of blood urea/nitrogen analyzer by input sample quality afterwards；
Perform analysis program in analysis software, blood urea/nitrogen analyzer is de-gassed set crucible in sample after processing automatically falls into
In crucible, the measurement of nitrogen impurity content in sample is completed, measurement result is calculated and be shown in blood urea/nitrogen analyzer automatically.
Step 1 and step 5 are repeated, carries out 6 measure altogether, measurement result is as follows：
Embodiment two the result shows that：The present invention measures nitrogen impurity content in MOX pellets, in the level that nitrogen content is 60 μ g/g
Under, precision is better than 5%.
Claims (10)
1. a kind of assay method of nitrogen content in MOX pellets, it is characterised in that：Include the following steps：
Step 1：Sample preparation
After MOX pellets sample progress physics is crushed, 0.050g~0.100g samples are weighed；
Step 2：Instrument prepares
1) before use, be switched on pre- more than thermal nitrogen analyzer 30min, and gas leakage detection is carried out after instrument stabilizer, and gas leakage detection passes through
Afterwards, acquiescence input sample quality is 1.000g, and n times skip test, 3≤N≤5 are carried out respectively using N number of empty graphite crucible, it is ensured that
The nitrogen content mass percent of blank, which is respectively less than, is equal to 0.0005%, and blank is without exception, and instrument is made to keep moderately good work
State；
2) setting blood urea/nitrogen analyzer analyzes power between 4900~5500W, and degassing power is between 5800~6200W, degassing time
Number is 2~3 times, and for degassing time between 30~50s, comparison level is 0.1~5.0%；
Step 3：Blank correction
M graphite crucible is respectively put into the nickel basket that the M specification of quality is 1g and carries out skip test, 3≤M≤5, acquiescence input
Sample quality is 1.000g, choose the three effective blank values of the nitrogen content mass percent of blank less than or equal to 0.001% into
Line blank corrects；
Step 4：Standard specimen corrects
The accurate quality for weighing 3~5 standard steel samples, mass value are accurate to 0.001g, are respectively charged into nickel basket, input standard steel
It measures after the quality of sample, using the measured value in the nitrogen content standard value range of standard steel sample as virtual value, is analyzing
Three virtual values are chosen in software to be corrected；
Step 5：Sample measures
Nickel basket equipped with sample is put into the measurement that nitrogen impurity content in sample is completed in blood urea/nitrogen analyzer, blood urea/nitrogen analyzer calculates automatically
And show measurement result.
2. the assay method of nitrogen content in a kind of MOX pellets as described in claim 1, it is characterised in that：The graphite earthenware
Crucible is set crucible.
3. the assay method of nitrogen content in a kind of MOX pellets as claimed in claim 2, it is characterised in that：In step 5, replace
After interior crucible in set crucible, set crucible is put under blood urea/nitrogen analyzer electrode furnace on electrode, then input sample quality, will be equipped with
The nickel basket of sample is put into the falling in sample sliding block of blood urea/nitrogen analyzer；
Analysis program is performed in analysis software, sample automatically falls into interior crucible after blood urea/nitrogen analyzer is de-gassed set crucible processing
In, the measurement of nitrogen impurity content in sample is completed, measurement result is calculated and be shown in blood urea/nitrogen analyzer automatically.
4. the assay method of nitrogen content in a kind of MOX pellets as claimed in claim 3, it is characterised in that：To same batch
Sample and single sample carry out parallel determination when, step 2~step 4 does not repeat.
5. the assay method of nitrogen content in a kind of MOX pellets as claimed in claim 4, it is characterised in that：Step 4 is weighing mark
Before quasi- steel sample, the nitrogen content in sample is estimated, the nitrogen content of the standard steel sample of selection should be close to the nitrogen quantity of tested sample, to carry
The accuracy of high measurement result.
6. the assay method of nitrogen content in a kind of MOX pellets as claimed in claim 5, it is characterised in that：In step 1, by MOX
Pellet sample is put into progress physics in agate mortar and crushes.
7. the assay method of nitrogen content in a kind of MOX pellets as claimed in claim 6, it is characterised in that：In step 1,
Sample fragment is added in the nickel basket weighed, weighs the nickel basket gross mass equipped with sample, sample quality is equal to the nickel basket equipped with sample
Gross mass subtracts nickel basket quality.
8. the assay method of nitrogen content in a kind of MOX pellets as claimed in claim 7, it is characterised in that：In step 2, setting
Blood urea/nitrogen analyzer analysis power is 5000W, and degassing power is 6000W, and degassing number is 2 times, degassing time 35s, comparison level
It is 1.0%.
9. the assay method of nitrogen content in a kind of MOX pellets as claimed in claim 8, it is characterised in that：It is in sample size
Under the conditions of 0.050g, the detection of this method is limited to 4.8 μ g/g；In the case where nitrogen content is the level of 60 μ g/g, precision is better than 5%.
10. such as the assay method of nitrogen content in a kind of MOX pellets of claim 1~9 any one of them, it is characterised in that：Institute
The blood urea/nitrogen analyzer stated is using inert gas high-temperature fusion-thermal conductivity method as measuring principle.
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Application publication date: 20180710 |