CN104020032A - Preparation method of test specimens for unbreakable ferro-vanadium chemical analysis - Google Patents
Preparation method of test specimens for unbreakable ferro-vanadium chemical analysis Download PDFInfo
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- CN104020032A CN104020032A CN201410271227.XA CN201410271227A CN104020032A CN 104020032 A CN104020032 A CN 104020032A CN 201410271227 A CN201410271227 A CN 201410271227A CN 104020032 A CN104020032 A CN 104020032A
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Abstract
The invention belongs to the field of ferrous alloy analysis, in particular relates to a preparation method of test specimens for ferrous alloy analysis, and particularly provides a preparation method of test specimens for unbreakable ferro-vanadium chemical analysis. In a preparation process of the test specimens, the grinding of a bowl material of a vibrating crusher and the degree of abrasion (dilution) of oxygen in air to the test specimens can be reduced, and the authenticity of vanadium content of the prepared test specimens and the preparation efficiency can be improved. The method specifically comprises the following steps of 1, cleaning equipment and appliances; 2, crushing large specimens until the granularity is not more than 10mm by using a jaw crusher, performing uniform mixing and division, reserving more than 2.0 kilograms of specimens, crushing the more than 2.0 kilograms of specimens until the granularity is not more than 5mm by using the jaw crusher, performing division, and reserving more than 0.5 kilograms of specimens; 3, crushing the more than 0.5 kilograms of specimens until all the specimens pass through 1.0-mm sieve meshes by using the vibrating crusher, performing division, and reserving more than 50 grams of specimens; and 4, treating the specimens until all the specimens pass through 0.250-mm sieve meshes, and performing uniform mixing to obtain the chemical analysis test specimens.
Description
Technical field
The invention belongs to ferroalloy analysis field, be specifically related to the preparation method of ferroalloy assay sample, a kind of preparation method who non-friable vanadium iron chemical analysis is used to sample is especially provided.
Background technology
Vanadium iron is because of impacts such as production technology difference and its impurity component content differences, and its sample is being prepared chemical analysis with in sample process, obviously has frangible and non-friable two kinds of vanadium iron, and wherein, non-friable vanadium iron has hardness greatly and the feature of higher toughness.Sample prepare representative aspect, at GB/T4010-1994 < < ferroalloy chemical analysis, with the taking and prepare in > > of sample, the preparation of vanadium iron sample is not proposed to control the representational measure of sample preparation.
Simultaneously, inventor finds that domestic and international laboratory, to preparing non-friable vanadium iron sample, oxygen contamination (dilution) sample shortage understanding or not enough to the seriousness understanding of this two point pollution (dilution) in comminutor material alms bowl material abrasive dust and air easily occurs, they generally pulverize non-friable vanadium iron sample with grindability and the poor comminutor of material alms bowl material wearing quality, in addition require in various degree sample to pass through 0.154mm, 0.125mm, 0.098mm ... the sieve apertures such as 0.063mm, inventor finds that above-mentioned disposal options and parameter control can cause sample granularity requirements meticulous, pulverize sample overlong time, cause material alms bowl material abrasive dust, in air, oxygen pollutes (dilution) sample in various degree, the problem that causes sample content of vanadium on the low side 0.6%～5%.Aspect sample preparation efficiency, standard GB/T4010-1994 ferroalloy chemical analysis with sample take and prepare in vanadium iron method for making sample, because of granularity reference mark too much (10mm, 5mm, 2.8mm, 1.0mm, 0.5mm) and the corresponding size sample division amount of keeping sample excessive (13.0kg, 2.0kg, 1.0kg, 0.4kg, 0.2kg) of broken sample process, thereby affect sample preparation speed; Separately, many laboratories adopt the non-friable vanadium iron sample of " manually break+vibrating pulverizer of hammer " or " jaw crusher+twin rollers+vibrating pulverizer " or " jaw crusher+disc mill+vibrating pulverizer " combination preparation, not only there is the problems such as personal injury hidden danger, noise is large, equipment failure rate is high, and sample preparation inefficiency.
The sample preparation technology that exploitation can overcome the problems referred to above is badly in need of in this area.
Summary of the invention
Technical matters solved by the invention is to provide a kind of preparation method who non-friable vanadium iron chemical analysis is used to sample, the method is in sample preparation process, can reduce the amount of oxygen contamination (dilution) sample in vibrating pulverizer material alms bowl material abrasive dust, air, improve the authenticity of made sample content of vanadium and improve sample preparation efficiency.
To achieve these goals, the concrete sample preparation step of the inventive method is:
The first step: cleaning equipment and utensil: appropriate with the same batch of vanadium iron sample of separately getting, clean successively sample making apparatus, utensil, and there is no obvious residual sample in checkout facility and utensil;
Second step: full-page proof is crushed to sample granularity with jaw crusher and is not more than 10mm, mix, division keeping sample >=2.0kg, then general >=2.0kg sample is crushed to granularity and is not more than 5mm, mixes division keeping sample >=0.5kg;
The 3rd step: sample >=0.5kg adopts vibrating pulverizer to pulverize, grinding time is not more than 1min, take out 1.0mm sieve aperture screening for sample, on sieve, remaining sample is pulverized again, grinding time is not more than 1min, takes out sample again with the screening of 1.0mm sieve aperture, until sample is all by 1.0mm sieve aperture, mix division keeping sample >=50g;
The 4th step: sample >=50g is first with the screening of 0.250mm sieve aperture, and on sieve, remaining sample is pulverized with vibrating pulverizer, and grinding time is not more than 1min, take out sample again with the screening of 0.250mm sieve aperture, until sample is all by 0.250mm sieve aperture, mix, be chemical analysis sample.
The present invention is for realizing in sample preparation process, reduce the amount of oxygen contamination (dilution) sample in vibrating pulverizer material alms bowl material abrasive dust, air, the authenticity this purpose that improves made sample content of vanadium shortens sample grinding time as far as possible, and its technical characterictic is:
1) select the vibrating pulverizer pulverizing sample that grindability is strong and material alms bowl material anti-wear performance is good.Its smashing capability requires: to 100g granularity be the non-friable vanadium iron sample of 1.0mm grinding time in 1.5min, can make sample all by 0.250mm sieve aperture.
2) pulverizing sample to granularity 0.250mm, first with 0.250mm mesh screen, separate and be less than 0.250mm sample, on sieve, sample is pulverized and is not more than 1min in limited time at every turn again.
3) sample granularity only limits the use of the control of sieving of 0.250mm sieve aperture, for avoiding the long period to pulverize sample, causes that content of vanadium is on the low side, should sample granularity not pulverized thinner.
Appropriate for getting with crowd vanadium iron sample 1-2kg with batch vanadium iron sample described in the first step in the inventive method.
Described in second step and the 3rd step, division adopts mechanical division or artificial division.Described division can adopt riffle method, conical quartering, grid division method, the conventional division methods such as glazing bar reduction device method or nine point samplings.The proportional contracting device of adoptable equipment.
It is potassium steel (Mn13), chrome molybdenum or tungsten carbide that the present invention adopts the material alms bowl material of described vibrating pulverizer.Found through experiments,, material alms bowl material strong at this preferred grindability is that the GJ-98-II type comminutor of potassium steel (Mn13) is prepared sample, and in the relative experiment of this type, the material alms bowl material abrasive dust of other type is minimum to sample effects.
Beneficial effect of the present invention is as follows:
1, sample prepare representative aspect: because of non-friable vanadium iron, to have hardness large, high tenacity feature, in preparing sample process, the grindability of conventional vibrating pulverizer a little less than, material alms bowl material anti-wear performance is poor, pulverize sample overlong time, cause the sample of expecting prepared by oxygen contamination in alms bowl material abrasive dust and air (dilution), make in sample content of vanadium on the low side, by selecting grindability stronger, the good vibrating pulverizer of material alms bowl material anti-wear performance, and take the measure of shortening pulverizing sample T.T. to prepare sample, achieve effective control sample is expected alms bowl material abrasive dust, the amount of oxygen contamination in air, thereby improve the representativeness of sample preparation.
2, aspect sample preparation efficiency: adopt jaw crusher to combine broken sample with vibrating pulverizer, in sample preparation process, sample granularity reference mark is few, and the division amount of keeping sample is not excessive, makes method for making sample have easy and simple to handle, sample preparation effect fast.
Embodiment
The embodiment of form, is described in further detail foregoing of the present invention again by the following examples, illustrates but does not limit the present invention.
Adopt following embodiment to screen the vibrating pulverizer of the difference material alms bowl that preparation method of the present invention uses, investigating the made granularity of preparation method of the present invention is the precision of 0.250mm sample and preparation method's degree of accuracy, and contrasts sample preparation efficiency with the method that standard GB/T4010-1994 records.
Embodiment mono-
The present embodiment is to be that FeV50 sample preparation becomes the method for sample for chemical analysis to the trade mark, and concrete preparation process is:
The first step: cleaning equipment and utensil: same crowd of vanadium iron sample 1～2kg with separately getting, cleans successively sample making apparatus, utensil, and there is no obvious residual sample in checkout facility and utensil.
Second step: full-page proof is crushed to sample granularity with jaw crusher and is not more than 10mm, mix, division keeping sample >=2.0kg, then general >=2.0kg sample is crushed to sample granularity with jaw crusher and is not more than 5.0mm, mixes division keeping sample >=0.5kg.
The 3rd step: sample >=0.5kg adopts vibrating pulverizer to pulverize, grinding time is not more than 1min, take out 1.0mm sieve aperture screening for sample, on sieve, remaining sample is pulverized again, grinding time is not more than 1min, takes out sample again with the screening of 1.0mm sieve aperture, until sample is all by 1.0mm sieve aperture, mix division keeping sample >=50g.
The 4th step: sample >=50g is first with the screening of 0.250mm sieve aperture, and on sieve, remaining sample is pulverized with vibrating pulverizer, and grinding time is not more than 1min, take out sample again with the screening of 0.250mm sieve aperture, until sample is all by 0.250mm sieve aperture, mix, be chemical analysis sample.
Embodiment bis-
The present embodiment is to be that FeV80 sample preparation becomes the method for sample for chemical analysis to the trade mark, and concrete preparation process is:
The first step: cleaning equipment and utensil: same crowd of vanadium iron sample 1～2kg with separately getting, cleans successively sample making apparatus, utensil, and there is no obvious residual sample in checkout facility and utensil.
Second step: full-page proof is crushed to sample granularity with jaw crusher and is not more than 10mm, mix, division keeping sample >=2.0kg, then general >=2.0kg sample is crushed to sample granularity with jaw crusher and is not more than 5.0mm, mixes division keeping sample >=0.5kg.
The 3rd step: sample >=0.5kg adopts vibrating pulverizer to pulverize, grinding time is not more than 1min, take out 1.0mm sieve aperture screening for sample, on sieve, remaining sample is pulverized again, grinding time is not more than 1min, takes out sample again with the screening of 1.0mm sieve aperture, until sample is all by 1.0mm sieve aperture, mix division keeping sample >=50g.
The 4th step: by sample >=50g, first, with the screening of 0.250mm sieve aperture, on sieve, remaining sample is pulverized and is not more than 1min with vibrating pulverizer, takes out sample again with the screening of 0.250mm sieve aperture, until sample is all by 0.250mm sieve aperture, mixes, and is chemical analysis sample.
Below investigating test is to adopt according to embodiment mono-, two preparation FeV50, FeV80 sample to test.
One, multiple vibrating pulverizer is prepared content of vanadium difference and the pollution effect test of different grain size sample
A. test vibrating pulverizer
The partial parameters of table 1 vibrating pulverizer
| Model | Material alms bowl material | Material alms bowl internal diameter/mm | Characteristic element content |
| GJ-98-Ⅱ | Potassium steel: Mn13 | 200 | Mn：12.04％ |
| GJ100-2 | Potassium steel: Mn13 | 140 | Mn：10.87％ |
| ZMF-1 | Chrome molybdenum | 140 | Cr：10.00％ |
| GJ-98-Ⅳ | Tungsten carbide | 125 | C：5.24％ |
B. test method:
A. sample: in advance FeV50 and FeV80 sample are crushed to respectively to granularity 1.0mm, mix, every group takes 5 parts of 100.0g samples, prepares 0.250mm, 0.177mm, 0.150mm, 0.125mm, 0.098mm sample respectively with different comminutors.
B. measure: to each Specimen Determination vanadium, characteristic element, oxygen content, the pollution level data of the content of vanadium difference of each comminutor different grain size sample, material alms bowl material abrasive dust, air oxygen are listed in table 2-9.△ V, △ V in table 2-9
m, △ V
o, △ V
xshown in as follows:
△ V---with respect to the variable quantity of 0.250mm granularity sample content of vanadium;
△ V
m---the abrasive dust amount increasing with respect to 0.250mm granularity sample affects the variable quantity of content of vanadium;
△ V
o---the oxygen amount increasing with respect to 0.250mm granularity sample affects the variable quantity of content of vanadium;
△ V
x---other factors causes the variable quantity of content of vanadium.
Table 2GJ-98-II type comminutor is prepared FeV50 sample the data obtained
Table 3GJ100-2 type comminutor is prepared FeV50 sample the data obtained
Table 4ZMF-1 type comminutor is prepared FeV50 sample the data obtained
Table 5GJ-98-IV type comminutor is prepared FeV50 sample the data obtained
Table 6GJ-98-II type comminutor is prepared FeV80 sample the data obtained
Table 7GJ100-2 type comminutor is prepared FeV80 sample the data obtained
Table 8ZMF-1 type comminutor is prepared FeV80 sample the data obtained
Table 9GJ-98-IV type comminutor is prepared FeV80 sample the data obtained
Test shows:
1) sample granularity is thinner, and sample grinding time is longer, and sample is expected, and in alms bowl material abrasive dust, air, oxygen contamination (dilution) is more serious, and sample content of vanadium is lower.
2) comminutor material alms bowl material anti-wear performance is better, and it is less that abrasive dust pollutes (dilution) amount, less on the impact of sample vanadium and other component content.
3) 0.250mm is less by abrasive dust, oxygen contamination (dilution) degree compared with 0.177mm sample, and sample preparation is representative better, and content of vanadium is more accurate.
4) in above-mentioned four kinds of types, GJ-98-II comminutor meets the smashing capability of technical characterictic requirement, prepared by non-friable vanadium iron to abrasive dust, the oxygen contamination of 0.250mm sample is little and pulverizing speed is fast, its sample preparation resultant effect is best, all uses this machine in following sample preparation.
Two, 0.250mm sample constituents is measured precision
By the embodiment of the present invention one, two record, by FeV50, each 30 batches of full-page proofs of FeV80 are prepared into the assay sample of granularity 0.250mm, and each sample is measured to vanadium V with different personnel, silicon Si, phosphorus P, aluminium Al, manganese Mn, carbon C, 2 parts of sulphur S content, add up the difference of 2 parts of measured values of each composition, each difference respectively with GB/T8704.5-2007: the mensuration-ferrous ammonium sulfate titration of vanadium iron-content of vanadium and potentiometric titration, GB/T8704.6-2007: mensuration-sulfuric acid determination of vanadium iron-silicone content, GB/T8704.7-2009: the mensuration-molybdenum blue spectrophotometric method of vanadium iron-phosphorus content, GB/T8704.8-2009: the mensuration-Chrome azurol s colorimetry of vanadium iron-aluminium content and EDTA titrimetry, GB/T8704.9-2009: mensuration-potassium metaperiodate photometry and the flame atomic absorption spectrometry of vanadium iron-manganese content, GB/T8704.1-2009: the mensuration-infrared absorption of vanadium iron-carbon content and gas volumetric method, GB/T8704.3-2009: the tolerance of the mensuration-infrared absorption of vanadium iron-sulfur content and burning acid-base titration law regulation is more not overproof.Test shows: the mensuration precision of each composition of 0.250mm granularity sample is good, can meet and measure requirement.
Three, the sample preparation degree of accuracy of assessment method for making sample
By the inventive method sample preparation, each 30 batches, every batch full-page proof amount of FeV50, FeV80 is no less than to 4kg, with jaw crusher, be crushed to granularity-10mm respectively, mix, division is 2 duplicate samples, by method of the present invention, 2 duplicate samples are prepared into sample 1 and the sample 2 that granularity is 0.250mm again, measure 2 parts of sample content of vanadium, count the sample preparation degree of accuracy β of FeV50, FeV80 content of vanadium
pbe respectively 0.228,0.305.Test shows: the sample preparation degree of accuracy β of the inventive method
pvalue is the β that takes and prepare > > with sample compared with GB/T4010-1994 < < ferroalloy chemical analysis all
p=0.4 is little, and the sample preparation degree of accuracy of the inventive method is good.
Four, the inventive method and the comparison of standard GB/T4010-1994 method sample preparation efficiency
With under " people, machine, sample " prerequisite, standard GB/T4010-1994 method and the inventive method complete the time that a 6kg full-page proof is prepared into sample and are respectively 29min, 14min, and the inventive method is easy, quick compared with the sample preparation of standard GB/T4010-1994 method.
To sum up compared with prior art, the inventive method has that sample preparation representativeness is good, degree of accuracy is high, easy, advantage and effect fast in test.
Claims (8)
1. the preparation method of sample for pair non-friable vanadium iron chemical analysis, is characterized in that: step is as follows:
The first step: cleaning equipment and utensil: separately get same batch vanadium iron sample appropriate, clean successively sample making apparatus, utensil, and there is no obvious residual sample in checkout facility and utensil;
Second step: full-page proof is crushed to sample granularity with jaw crusher and is not more than 10mm, mix, division keeping sample >=2.0kg, then general >=2.0kg sample is crushed to sample granularity with jaw crusher and is not more than 5.0mm, mixes division keeping sample >=0.5kg;
The 3rd step: sample >=0.5kg adopts vibrating pulverizer to pulverize, grinding time is not more than 1min, take out 1.0mm sieve aperture screening for sample, on sieve, remaining sample is pulverized again, grinding time is not more than 1min, takes out sample again with the screening of 1.0mm sieve aperture, until sample is all by 1.0mm sieve aperture, mix division keeping sample >=50g;
The 4th step: sample >=50g is first with the screening of 0.250mm sieve aperture, and on sieve, remaining sample is pulverized with vibrating pulverizer, and grinding time is not more than 1min, take out sample again with the screening of 0.250mm sieve aperture, until sample is all by 0.250mm sieve aperture, mix, be chemical analysis sample.
2. the preparation method who non-friable vanadium iron chemical analysis is used to sample according to claim 1, is characterized in that: described in the first step, with batch vanadium iron sample, states with criticizing vanadium iron sample 1-2kg in right amount for getting.
3. the preparation method who non-friable vanadium iron chemical analysis is used to sample according to claim 1, is characterized in that: described in second step and the 3rd step, division adopts mechanical division or artificial division.
4. the preparation method who non-friable vanadium iron chemical analysis is used to sample according to claim 1, is characterized in that: described in second step and the 3rd step, division adopts riffle method, conical quartering, grid division method, glazing bar reduction device method or nine point samplings.
5. the preparation method who non-friable vanadium iron chemical analysis is used to sample according to claim 1, is characterized in that: division adoption rate contracting device described in second step and the 3rd step.
6. the preparation method who non-friable vanadium iron chemical analysis is used to sample according to claim 1, is characterized in that: the material alms bowl material of described vibrating pulverizer is potassium steel, chrome molybdenum or tungsten carbide.
7. the preparation method who non-friable vanadium iron chemical analysis is used to sample according to claim 6, is characterized in that: the material alms bowl material of described vibrating pulverizer is potassium steel Mn13.
According to claim 1 to non-friable vanadium iron chemical analysis the preparation method with sample, it is characterized in that: adopt the vibrating pulverizer with following grindability: to 100g granularity, be that the non-friable vanadium iron sample of 1.0mm is pulverized in 1.5min, can make sample all by 0.250mm sieve aperture.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104458372A (en) * | 2014-11-28 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Sample preparation method of mixed material containing soft metal |
| CN107345871A (en) * | 2017-06-30 | 2017-11-14 | 广西贺州市科隆粉体有限公司 | A kind of calcium carbonate material quality detection method |
| CN107389397A (en) * | 2017-06-30 | 2017-11-24 | 包头钢铁（集团）有限责任公司 | A kind of preparation method of manganese metal chemical analysis sample |
| CN107589107A (en) * | 2015-03-30 | 2018-01-16 | 国核宝钛锆业股份公司 | Method that is a kind of while determining beryllium potassium content in zirconium and zircaloy |
| CN107870107A (en) * | 2017-11-13 | 2018-04-03 | 中国铝业股份有限公司 | A kind of method for making sample of iron ore concentrate |
| CN110118792A (en) * | 2018-02-07 | 2019-08-13 | 腾达西北铁合金有限责任公司 | A kind of pressed powder method for making sample of ferroalloy productor and raw material |
| CN111197141A (en) * | 2020-02-21 | 2020-05-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Control method for fine powder rate of FeV50 alloy |
| CN111707518A (en) * | 2020-07-21 | 2020-09-25 | 广东韶钢松山股份有限公司 | Sample for chemical analysis of low-carbon ferrochrome and sample preparation method |
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Cited By (11)
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| CN104458372A (en) * | 2014-11-28 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Sample preparation method of mixed material containing soft metal |
| CN107589107A (en) * | 2015-03-30 | 2018-01-16 | 国核宝钛锆业股份公司 | Method that is a kind of while determining beryllium potassium content in zirconium and zircaloy |
| CN107589107B (en) * | 2015-03-30 | 2020-04-28 | 国核宝钛锆业股份公司 | Method for simultaneously determining beryllium and potassium content in zirconium and zirconium alloy |
| CN107345871A (en) * | 2017-06-30 | 2017-11-14 | 广西贺州市科隆粉体有限公司 | A kind of calcium carbonate material quality detection method |
| CN107389397A (en) * | 2017-06-30 | 2017-11-24 | 包头钢铁（集团）有限责任公司 | A kind of preparation method of manganese metal chemical analysis sample |
| CN107345871B (en) * | 2017-06-30 | 2020-06-19 | 广西贺州市科隆粉体有限公司 | Calcium carbonate raw material quality detection method |
| CN107870107A (en) * | 2017-11-13 | 2018-04-03 | 中国铝业股份有限公司 | A kind of method for making sample of iron ore concentrate |
| CN110118792A (en) * | 2018-02-07 | 2019-08-13 | 腾达西北铁合金有限责任公司 | A kind of pressed powder method for making sample of ferroalloy productor and raw material |
| CN111197141A (en) * | 2020-02-21 | 2020-05-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Control method for fine powder rate of FeV50 alloy |
| CN111197141B (en) * | 2020-02-21 | 2021-01-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Control method for fine powder rate of FeV50 alloy |
| CN111707518A (en) * | 2020-07-21 | 2020-09-25 | 广东韶钢松山股份有限公司 | Sample for chemical analysis of low-carbon ferrochrome and sample preparation method |
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