CN104316345A - Multi-component rare earth raw material sampling method - Google Patents
Multi-component rare earth raw material sampling method Download PDFInfo
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- CN104316345A CN104316345A CN201410497286.9A CN201410497286A CN104316345A CN 104316345 A CN104316345 A CN 104316345A CN 201410497286 A CN201410497286 A CN 201410497286A CN 104316345 A CN104316345 A CN 104316345A
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Abstract
The invention discloses a multi-component rare earth raw material sampling method. The rare earth raw materials comprise lanthanum-cerium alloy, cell-grade mixed rare earth and a multi-component rare earth alloy composed of two or more rare earth elements. The rare earth raw materials are metals in as-cast state, have clean surfaces and no obvious oxide layers and form metal alloy ingots without obvious included slag. The multi-component rare earth raw material sampling method comprises determining sampling number according to a material detail form provided by a supplier and the number of one batch of fed materials, taking samples by a drill bit, weighing the samples according to the material detail form provided by the supplier, combining the samples to form an integrated sample, pre-treating the integrated sample and detecting ingredients of the multi-component rare earth alloy. The multi-component rare earth raw material sampling method has the advantages that the taken sample is representative, the detection result is real and reliable and production burdening is accurate.
Description
Technical field
The present invention relates to a kind of methods of sampling of polycomponent terres rares raw material, the polycomponent rare earth alloy that described terres rares raw material comprises lanthanum cerium alloy, cell-grade mixed rare earth and is made up of two or more rare earth element; Described terres rares raw material is as cast condition shape metal, clean surface, and without obvious oxide layer, metal alloy ingot is without obvious slag inclusion.This terres rares raw material is the hydrogen storing alloy powder use for nickel-hydrogen battery, and hydrogen bearing alloy is a kind of can absorption under certain condition and releasing hydrogen gas, the material with reversible hydrogen adsorption and desorption performance.
Background technology
At present, the sampling method of polycomponent terres rares raw material, for often entering a collection of terres rares raw material gets 4-7 sample, during weight≤500 Kg often criticized, gets 4 samples.Often increase 500kg to add and get a sample, maximum 7, sampling shortcoming is like this that got sample does not have representativeness, because often sometimes the composition difference of each barrel of different masses sample is very large, if during supplied materials in enormous quantities, only get 7 meetings and cause a lot of raw material to be in the state of lapsing.
Summary of the invention
The object of this invention is to provide a kind of methods of sampling of polycomponent terres rares raw material, time especially for supplied materials in enormous quantities, make got sample have more representativeness, the result surveyed is closer to its actual value.
For this reason, the invention provides a kind of methods of sampling of polycomponent terres rares raw material, the polycomponent rare earth alloy that described terres rares raw material comprises lanthanum cerium alloy, cell-grade mixed rare earth and is made up of two or more rare earth element; Described terres rares raw material is as cast condition shape metal, clean surface, and without obvious oxide layer, metal alloy ingot is without obvious slag inclusion; The step of the described methods of sampling comprises:
1. determine to sample number according to supplier's material detail form and a batch of supplied materials quantity;
A, a described batch of supplied materials quantity are n(n is integer, if n >=1) ton, total total n small batch, namely each small batch is 1 ton, at least uses 4 barreleds for every 1 ton, supplier's material detail form shows n group and detects data; Then every 1 small batch gets 3 barrels, gets a sample for every barrel, and three samples of each small batch sample rear composition comprehensive sample in the ratio of 1:1:1, a batch of comprehensive sample of n altogether;
B, a described batch of supplied materials quantity are n(n is integer, if 1 < n < 5) ton, at least use 4 barreleds for every 1 ton, namely on supplier's material detail form, only display one group detects data; Then get 4 barrels of supplied materials at random, get a sample for every barrel, every two samples sample rear composition comprehensive sample in the ratio of 1:1, altogether 2 comprehensive samples;
C, a described batch of supplied materials are n(n is integer, if n >=5) ton, namely on supplier's material detail form, only display one group detects data; Then get (4+2n/5) (rounding numerical digit) bucket supplied materials at random, get a sample for every barrel, every two samples sample rear composition comprehensive sample in the ratio of 1:1, total total individual comprehensive sample of (2+n/5) (rounding numerical digit).
2. bit drills is adopted to materials; Adopt diameter 6mm-10mm drill bit to drill through the upper and lower surface of alloy pig, each more than 3, brill, sample drills through degree of depth 8-10mm, discards the drilling cuttings apart from surperficial 0.5-1.0mm, then will drill through sample and load immediately in sampling bag.
3. the comprehensive sample of composition (2+n/5) (rounding numerical digit) after sample being weighed according to supplier's material detail form.
Pre-treatment is carried out to comprehensive sample: take sample and be placed in beaker, add the nitric acid of 1:1, move in 100 ml volumetric flasks after dissolving, be diluted with water to 100 ml, shake up; Get test solution 5ml in 50 ml volumetric flasks with transfer pipet, be diluted with water to 50 ml, shake up to be measured.
4. the component of polycomponent rare earth alloy is detected; The component of described detection polycomponent rare earth alloy is that the detecting instrument by comprising inductively coupled plasma atomic emission spectrometer (ICP-AES) detects.
The invention has the beneficial effects as follows: the sample got has more representativeness, the result surveyed is more true and reliable, and it is more accurate to be convenient to produce batching.
Accompanying drawing explanation
Fig. 1 is the sampling flowsheet figure of the methods of sampling according to polycomponent terres rares raw material of the present invention.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.
embodiment 1:a methods of sampling for lanthanum cerium mischmetal raw metal, as shown in Figure 1; One batch of lanthanum cerium mischmetal raw metal, weight is 10 tons, always has 10 small batches, and namely each small batch is 1 ton, every 1 ton of use 4 barreleds, and supplier's material detail form has 10 groups to detect data.Every 1 ton namely each small batch get 3 barrels, get a sample for every barrel, to three alloy pig samples of each small batch, materials by 7mm bit drills, discard the drilling cuttings apart from surperficial 0.5-1.0mm, then will drill through sample and load immediately in sampling bag; After sampling in the ratio of 1:1:1 subsequently, form a comprehensive sample, altogether 10 comprehensive samples.After comprehensive sample pre-service, detect with ICP-AES spectrometer.
In order to prove practicality and the reliability of this method, sampling inspection results contrast being carried out to this batch of lanthanum ce metal raw material Conventional sampling methods and sampling method of the present invention, lists in table 1.Wherein A represents conventional method, and B represents sampling method of the present invention, and 1-10 represents 10 small batches.To measure the result difference come larger for two kinds of sampling methods as can be seen from Table 1; Illustrate that the composition difference of each barrel of different masses sample is very large, so the sample that A method is got does not have representativeness, and have part material to be in the state of lapsing, and of the present invention what get is comprehensive sample, and each has sampling in small batches, institute's sample thief has more representativeness, therefore, the test result that sampling method of the present invention draws is more true and reliable, and in production, batching is more accurate.
Table 1 two kinds of methods of sampling testing result contrast tables
| Element | La/Re | Ce/Re | Pr/Re | Nd/Re | Fe | Mg |
| A1 | 31.71 | 68.10 | 0.0618 | 0.1267 | 0.1400 | 0.0010 |
| B1 | 35.75 | 64.11 | 0.0496 | 0.0868 | 0.1267 | 0.0069 |
| Difference | 4.04 | 3.99 | 0.0122 | 0.0399 | 0.0133 | 0.0059 |
| A2 | 34.77 | 65.12 | 0.0411 | 0.0721 | 0.1050 | 0.0100 |
| B2 | 36.23 | 63.65 | 0.0439 | 0.0744 | 0.1403 | 0.0076 |
| Difference | 1.46 | 1.47 | 0.0028 | 0.0023 | 0.0007 | 0.0024 |
| A3 | 34.79 | 65.10 | 0.0377 | 0.0696 | 0.0597 | 0.0017 |
| B3 | 36.78 | 63.06 | 0.0440 | 0.0740 | 0.0748 | 0.0197 |
| Difference | 1.99 | 2.04 | 0.0063 | 0.0044 | 0.0151 | 0.0180 |
| A4 | 35.71 | 64.17 | 0.0420 | 0.0823 | 0.2375 | 0.0018 |
| B4 | 34.70 | 65.17 | 0.0454 | 0.0818 | 0.1364 | 0.0080 |
| Difference | 1.01 | 1.00 | 0.0034 | 0.0005 | 0.1011 | 0.0062 |
| A5 | 35.32 | 64.57 | 0.0443 | 0.0655 | 0.1952 | 0.0010 |
| B5 | 35.13 | 64.76 | 0.0426 | 0.0692 | 0.0748 | 0.0070 |
| Difference | 0.19 | 0.19 | 0.0017 | 0.0037 | 0.1204 | 0.006 |
| A6 | 32.72 | 67.16 | 0.0454 | 0.0792 | 0.1387 | 0.0059 |
| B6 | 37.10 | 62.79 | 0.0397 | 0.0676 | 0.0532 | 0.0052 |
| Difference | 4.38 | 4.37 | 0.0057 | 0.0116 | 0.0855 | 0.0007 |
| A7 | 35.10 | 64.78 | 0.0403 | 0.0778 | 0.1497 | 0.0061 |
| B7 | 36.60 | 63.28 | 0.0395 | 0.0738 | 0.0600 | 0.0095 |
| Difference | 1.50 | 1.50 | 0.0008 | 0.0040 | 0.0897 | 0.0034 |
| B8 | 34.46 | 65.46 | 0.0434 | 0.0797 | 0.0920 | 0.0113 |
| B9 | 33.63 | 66.27 | 0.0430 | 0.0566 | 0.1607 | 0.0054 |
| B10 | 36.64 | 63.25 | 0.0401 | 0.0713 | 0.1552 | 0.0081 |
embodiment 2:a methods of sampling for lanthanum cerium mischmetal raw metal, as shown in Figure 1; If supplied materials 5 tons, and 5 tons of raw materials are one batch, at least use 4 barreleds for every 1 ton, and on supplier's material detail form, only display one group detects data; Then get 6 barrels of supplied materials at random, get a sample for every barrel, to 6 alloy pig samples, materials by 8mm bit drills, discard the drilling cuttings apart from surperficial 0.5-1.0mm, then will drill through sample and load immediately in sampling bag; Every two samples sample rear composition comprehensive sample in the ratio of 1:1, altogether 3 comprehensive samples.After comprehensive sample pre-service, detect with ICP-AES spectrometer.
embodiment 3:a methods of sampling for lanthanum cerium mischmetal raw metal, as shown in Figure 1; If supplied materials 12 tons, and 12 tons of raw materials are one batch, at least use 4 barreleds for every 1 ton, and on supplier's material detail form, only display one group detects data; Then get 8 barrels of supplied materials at random, get a sample for every barrel, to 8 alloy pig samples, materials by 9mm bit drills, discard the drilling cuttings apart from surperficial 0.5-1.0mm, then will drill through sample and load immediately in sampling bag; Every two samples sample rear composition comprehensive sample in the ratio of 1:1, altogether 6 comprehensive samples.After comprehensive sample pre-service, detect with ICP-AES spectrometer.
embodiment 4:describedly pre-treatment is carried out to comprehensive sample comprise: accurately take 0.1000g sample and be placed in 100ml beaker, after adding 10 ml nitric acid dissolves, move into 100 ml volumetric flasks, be diluted with water to 100 ml scales, shake up.Get above-mentioned test solution 5ml in 50 ml volumetric flasks with transfer pipet, be diluted with water to 50 ml scales, shake up to be measured.Nitric acid used and the volume ratio of water are 1:1.
Claims (6)
1. a methods of sampling for polycomponent terres rares raw material, the polycomponent rare earth alloy that described terres rares raw material comprises lanthanum cerium alloy, cell-grade mixed rare earth and is made up of two or more rare earth element; Described terres rares raw material is as cast condition shape metal, clean surface, and without obvious oxide layer, metal alloy ingot is without obvious slag inclusion; The step of the described methods of sampling comprises:
1. determine to sample number according to supplier's material detail form and a batch of supplied materials quantity;
2. bit drills is adopted to materials;
3. the comprehensive sample of composition after sample being weighed according to supplier's material detail form;
4. pre-treatment is carried out to comprehensive sample;
5. the component of polycomponent rare earth alloy is detected.
2. the methods of sampling of polycomponent terres rares raw material according to claim 1, is characterized in that:
A, a described batch of supplied materials quantity are n(n is integer, if n >=1) ton, total total n small batch, namely each small batch is 1 ton, at least uses 4 barreleds for every 1 ton, supplier's material detail form shows n group and detects data; Then every 1 small batch gets 3 barrels, gets a sample for every barrel, and three samples of each small batch sample rear composition comprehensive sample in the ratio of 1:1:1, a batch of comprehensive sample of n altogether;
B, a described batch of supplied materials quantity are n(n is integer, if 1 < n < 5) ton, at least use 4 barreleds for every 1 ton, namely on supplier's material detail form, only display one group detects data; Then get 4 barrels of supplied materials at random, get a sample for every barrel, every two samples sample rear composition comprehensive sample in the ratio of 1:1, altogether 2 comprehensive samples;
C, a described batch of supplied materials are n(n is integer, if n >=5) ton, namely on supplier's material detail form, only display one group detects data; Then get (4+2n/5) (rounding numerical digit) bucket supplied materials at random, get a sample for every barrel, every two samples sample rear composition comprehensive sample in the ratio of 1:1, total total individual comprehensive sample of (2+n/5) (rounding numerical digit).
3. the methods of sampling of polycomponent terres rares raw material according to claim 1, it is characterized in that: it is the upper and lower surface adopting diameter 6mm-10mm drill bit to drill through alloy pig that described bit drills is materialsed, more than 3, each brill, sample drills through degree of depth 8-10mm, discard the drilling cuttings apart from surperficial 0.5-1.0mm, then will drill through sample and load immediately in sampling bag.
4. the methods of sampling of the polycomponent terres rares raw material according to claims 1 or 2, is characterized in that: the individual comprehensive sample of composition (2+n/5) (rounding numerical digit) after being weighed by sample according to supplier's material detail form.
5. the methods of sampling of polycomponent terres rares raw material according to claim 1, is characterized in that:
Describedly pre-treatment is carried out to comprehensive sample comprise: take sample and be placed in beaker, add the nitric acid of 1:1, move in 100 ml volumetric flasks after dissolving, be diluted with water to 100 ml, shake up; Get test solution 5ml in 50 ml volumetric flasks with transfer pipet, be diluted with water to 50 ml, shake up to be measured.
6. the methods of sampling of polycomponent terres rares raw material according to claim 1, is characterized in that:
The component of described detection polycomponent rare earth alloy is that the detecting instrument by comprising inductively coupled plasma atomic emission spectrometer (ICP-AES) detects.
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| CN111855268A (en) * | 2020-07-14 | 2020-10-30 | 武汉华科新材料有限公司 | Processing method for analyzing test sample by using coring to drill oxygen, nitrogen and hydrogen |
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| CN111855268A (en) * | 2020-07-14 | 2020-10-30 | 武汉华科新材料有限公司 | Processing method for analyzing test sample by using coring to drill oxygen, nitrogen and hydrogen |
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