CN104964941B - Method and separating and collecting device for detecting elemental selenium quickly and quantitatively - Google Patents
Method and separating and collecting device for detecting elemental selenium quickly and quantitatively Download PDFInfo
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 238000000034 method Methods 0.000 title abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 27
- 239000005388 borosilicate glass Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims description 18
- 241000251468 Actinopterygii Species 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 abstract description 13
- 239000007864 aqueous solution Substances 0.000 abstract description 11
- 229910052979 sodium sulfide Inorganic materials 0.000 abstract description 8
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 abstract 2
- 230000006698 induction Effects 0.000 abstract 1
- 239000011669 selenium Substances 0.000 description 65
- 229940091258 selenium supplement Drugs 0.000 description 45
- 229910052711 selenium Inorganic materials 0.000 description 43
- 239000000523 sample Substances 0.000 description 23
- 239000000126 substance Substances 0.000 description 12
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 9
- 239000011734 sodium Substances 0.000 description 8
- 238000002835 absorbance Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000012224 working solution Substances 0.000 description 6
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 229940065287 selenium compound Drugs 0.000 description 4
- 150000003343 selenium compounds Chemical class 0.000 description 4
- 229960001471 sodium selenite Drugs 0.000 description 4
- 239000011781 sodium selenite Substances 0.000 description 4
- 235000015921 sodium selenite Nutrition 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000222065 Lycoperdon Species 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 241000768494 Polymorphum Species 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003674 animal food additive Substances 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000010959 commercial synthesis reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000000559 atomic spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012472 biological sample Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000816 toxic dose Toxicity 0.000 description 1
- -1 vitriolization Chemical compound 0.000 description 1
- 238000000209 wet digestion Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method and separating and collecting device for detecting elemental selenium quickly and quantitatively. The method comprises the steps that 1 a standard curve is drew; 2 a sample of the elemental selenium to be tested is placed into the separating and collecting device, heating is conducted at the temperature of 300 DEG C for 30 min on a heating plate of an induction cooker, collected selenium powder is transferred to a volumetric flask through 1M Na2S aqueous solution after cooling is conducted, the solution is taken out after the volume is metered, and the absorption value is measured through an ultraviolet spectrohoptometer when the absorption wavelength is 500 mm. The separating and collecting device is made of borosilicate glass materials. The separating and collecting device comprises a glass base and an upper cover cavity. A polishing skirt is arranged at the glass base. A polishing skirt is arranged at the bottom of the upper cover bottom correspondingly. An air set pipe is arranged at the top portion of the upper cover cavity. A vertical line of the air set pipe and the upper cover cavity is stretched out with an inclined angle of 120 degrees and is extended vertically and downward. The method and separating and collecting device for detecting elemental selenium quickly and quantitatively have the advantages that the elemental selenium is separated with other impurities, and the elemental selenium is collected; the operation is simple and accurate, the cost is low, and replicability is strong.
Description
Technical field
The present invention relates to a kind of method of Quantitative detection elemental selenium and separate and collect device.
Background technology
Selenium has four kinds of redox states:Se(VI)、Se(IV)、Se(-II)And Se(0), Se(VI)And Se(IV)Typically
Existed with inorganic form such as selenate and selenites.Se(-II)It is commonly referred to as organic selenium, be present in protein(Chen,
2006).Se(0)It is red or Lycoperdon polymorphum Vitt powder, with the metalloid of grey metal gloss.
Elemental selenium can be obtained by commercial synthesis, also can be obtained the selenium reduction of oxidation state by antibacterial(Tugarova, 2014;
Liu, 2014), the red elemental selenium particle diameter that commercial synthesis or bioconversion obtain is less, is also called nanometer selenium, usually by zero
The particle diameter that valency selenium is made red nano material within 60 ~ 80 nm(Chen Hui, 2006;Fu Xuefeng, 2008;Dobias, 2011).
The catalogue of feed additive varieties of China(2013)Middle sodium selenite and yeast selenium are added as mineral element feedstuff
Plus agent is used for cultivated animals Selenium supplement agent.Sodium selenite enriches as selenium additive, selenium source, and price is relatively low, but there is biology and have
Between low, toxic dose and requirement, scope is little, toxicity is big, easily pollute the defects such as environment for effect property, thus is strictly limited its use
Amount(Liu Heng, 2014), some countries and regions such as European Union have limited or have prohibitted the use of sodium selenite as the nutritional supplementation of selenium
Agent(Liu Na, 2010).Yeast selenium is increasingly considered to be preferable selenium-replenishing preparation and Ying Yu animal feeding
(Schrauzer, 2006).And almost meanwhile, nanometer selenium is because causing the advantages of its high bioavailability and hypotoxicity
Widely studied(Hu Caihong, 2007;Zhu Fenghua, 2010;Chen Jianjie, 2013).There are some researches show, with respect to sodium selenite, seleno
The selenium supplement product such as Methionine, nanometer selenium not only has more preferable absorption efficiency, and toxicity is lower(Wang, 2007;Zhang,
2008).The biological effectiveness of selenium and toxicity are closely related with its chemical form and content.Therefore, set up feed additive
In selenium element morphological analyses and its content analysis method, for feed safety control with assessment of nutritional value there is important meaning
Justice.
At present, total selenium assay method relative maturity.Mainly there is atomic spectroscopy(Najafi, 2010), inductive mass spectrum
Method(Zhong Na, 2013), ultraviolet spectrophotometry(Gong, 2005), fluorescence spectrophotometry(Koike, 1993), high-efficient liquid phase color
Spectrometry(Terumichi, 1989), gas chromatography(Nahid, 2012)Deng.In above-mentioned analysis method pretreatment process, sample is equal
Must first carry out in acid condition wet clear up, the selenium in sample is unified oxidoreduction and is become tetravalence selenium, more straight by above-mentioned instrument
Connect or indirectly tetravalence selenium is detected.Selenium because of all forms in sample there occurs that oxidoreduction is anti-in wet digestion process
Should, finally what detection obtained is the content of total selenium in sample.For the assay method of inorganic selenium, document report is first with slow
Rush salt or acid to extract(Gao Jianzhong, 2006), then take the assay method of total selenium to be measured, have the total selenium of document report and
The difference of inorganic selenium is organic selenium(Gao Jianzhong, 2006;DB, 2007)But, for specific sample, minusing obtains
Be Se(-II)And Se(0)Summation(Chen, 2006).So far, how Se in detection sample(-II)And Se(0)It is one
An individual difficult problem.For elemental selenium detection, progress is slow.Elemental selenium is water insoluble, alcohol, vitriolization, nitric acid, curing
Carbon;Sodium sulfite and sodium sulfide etc. can not optionally dissolve elemental selenium, thus specified rate analysis brings the problem of matrix interference;
Dissolubility in Carbon bisulfide for the selenium is relatively low, and its dissolubility in Carbon bisulfide of document report only has 0.64 mg/ml(Chen,
2006), bring difficulty to the extraction of Selenium In Some Selenium-rich Biological Samples, next to that Carbon bisulfide is poisonous, should avoid using in the lab as far as possible.Mesh
Before, great majority, for the research of elemental selenium, are mainly based upon the qualitative or sign that X-ray, scanning electron microscope or transmission electron microscope are carried out
Analysis(Kessi, 1999;Dhanjal, 2010;Rashimi, 2011).Only minority paper is related to the quantitative determination of elemental selenium
(Velinsky, 1990;Chen, 2006).Wherein Keka(Keka, 2011)Report adopts 1 M Na2S extraction with aqueous solution antibacterial gives birth to
The nanometer selenium of thing synthesis, more directly measures through ultraviolet spectrophotometry, but actually extraction be not only Se(0), also include
The Se of other valence states, and other substrate in sample, thus cause testing result to be significantly larger than the actual content of elemental selenium.
Determined by ultraviolet spectrophotometry is easily disturbed, and brings uncertain error.For elemental selenium detection there is no at present maturation,
Reliable, method with low cost.
Dry ashing method is common heavy metal in national standard method and the pre-treating method of non-metal kind Element detection
(GB/T 5009.11-2003), but not yet it is used for process and the mensure of elemental selenium.
Content of the invention
The needs of elemental selenium content detection in shortage for existing elemental selenium detection technique and actual Feed Sample, this
Invention provides a kind of method of Quantitative detection elemental selenium and separates and collects device.
A kind of method of Quantitative detection elemental selenium,
1)The drafting of standard curve
Weigh elemental selenium standard substance and be dissolved in 1M Na2In S, obtain the selenium standard working solution of multiple variable concentrations, using ultraviolet
The absorbance when absorbing wavelength is 500 nm for the spectrophotometer measurement selenium standard working solution, obtains standard curve;
2)Elemental selenium sample to be measured is inserted to be separated and collected in device, in the heating plate of electromagnetic oven, 300 DEG C of heating 30
Min, uses 1M Na after cooling2The selenium powder of collection is transferred to volumetric flask by S aqueous solution, takes out solution and utilize ultraviolet spectrometry after constant volume
Photometer measurement absorbing wavelength is absorbance during 500 nm;Comparison step 1)Standard curve after, obtain elemental selenium to be measured
The simple substance Se content of sample.
Described elemental selenium sample to be measured contains organic substance and oxidation state selenium compound and elemental selenium.
Described elemental selenium sample to be measured is Feed Sample.
A kind of Quantitative detection elemental selenium separate and collect device, using borosilicate glass material, including glass
Base, upper lid cavity, glass base is provided with ground shirt rim, and the bottom of upper lid cavity is provided with the ground shirt rim accordingly coincideing, on
The top of lid cavity is provided with an air set pipe, and described air set pipe is stretched out for 120 degree with angle with the vertical line of upper lid cavity
Extend vertically downward more afterwards.
Described glass base, upper lid cavity are symmetrically fixed using fish tail folder.
Described glass base, upper lid cavity, the thickness of glass of air set pipe are 0.3 cm.
Described glass base inner diameter is 2.3 cm, high 1 cm, wide 1.2 cm in ground shirt rim;Upper lid cavity ground shirt rim
Wide 1.2 cm, cavity internal diameter 2.3 cm, high 7 cm, air setting bore 0.5 cm, total length 30 cm, wherein 120 degree angles
Extend 10 cm vertically downward after extending 20 cm.
Described glass base is used for placing elemental selenium to be measured and heats on hot plate.
Beneficial effects of the present invention:
In heating process, destroyed after Organic substance calcination, the selenium such as Se of oxidation state(VI)And Se(IV)Salt can not be steamed
Send out, stay a glass bottom, and elemental selenium is volatilized as a vapor because its fusing point is low and condenses and is attached to upper lid inwall or air is cold
The inwall of solidifying pipe.Heating process had both separated elemental selenium and other impurities, so that elemental selenium is enriched with;Heat time heating time is shorter,
30 min can complete;This device materials is borosilicate glass, heat-resisting, and cost is relatively low, is easy to popularize;Heater is general
Logical temperature control electromagnetic oven is so that common lab can complete separation and the enrichment of elemental selenium with the method.Present invention operation letter
Single accurate, low cost, reproducibility is strong.
Brief description
The present invention is described in more detail with reference to the accompanying drawings and detailed description;
Fig. 1 is the pictorial diagram separating and collecting device of Quantitative detection elemental selenium(Left part is divided into glass bottom seat, right part
It is divided into lid cavity);
Fig. 2 is the schematic diagram separating and collecting device of Quantitative detection elemental selenium(Left part is divided into glass bottom seat, right part
It is divided into lid cavity);
Fig. 3 is standard curve and the linear equation of selenium standard solution.
Specific embodiment
Dry ashing method is generally used for the pre-treatment of high-melting-point sample analysis, and its operating procedure is that solid sample first carries out carbon
Change, then sample is put in Muffle furnace be ashed, ash residue is as analysis determinand(GB/T 5009.11-2003).
The fusing point of elemental selenium is 217 DEG C, is not suitable for collecting ash residue the elemental selenium it is contemplated that mentioning in background technology
Mensure problem, we attempt in heating process collect selenium steam, organic substance and oxidation state selenium compound are avoided with this
Interference.There is no the device collecting selenium steam in heating process in the market, so we devise a kind of device, in addition carry
Go out the directly related property between instrumental response value and the concentration based on selenium, the method for quantitative analyses simple substance Se content.
A kind of method of Quantitative detection elemental selenium,
1)The drafting of standard curve
Weigh elemental selenium standard substance and be dissolved in 1M Na2In S, obtain the selenium standard working solution of multiple variable concentrations, using ultraviolet
The absorbance when absorbing wavelength is 500 nm for the spectrophotometer measurement selenium standard working solution, obtains standard curve;
2)Elemental selenium sample to be measured is inserted to be separated and collected in device, in the heating plate of electromagnetic oven, 300 DEG C of heating 30
Min, uses 1M Na after cooling2The selenium powder of collection is transferred to volumetric flask by S aqueous solution, takes out solution and utilize ultraviolet spectrometry after constant volume
Photometer measurement absorbing wavelength is absorbance during 500 nm;Comparison step 1)Standard curve after, obtain elemental selenium to be measured
The simple substance Se content of sample.
Described elemental selenium sample to be measured contains organic substance and oxidation state selenium compound and elemental selenium.
Described elemental selenium sample to be measured is Feed Sample.
As shown in Figure 1, 2, a kind of Quantitative detection elemental selenium separate and collect device, using borosilicate glass material
Matter, including glass base, upper lid cavity, glass base is provided with ground shirt rim, and the bottom of upper lid cavity is provided with and accordingly coincide
Ground shirt rim, the top of upper lid cavity is provided with an air set pipe, the vertical line of described air set pipe and upper lid cavity with
120 degree of angle extends after stretching out vertically downward again.
Described glass base, upper lid cavity are symmetrically fixed using fish tail folder.
Described glass base, upper lid cavity, the thickness of glass of air set pipe are 0.3 cm.
Described glass base inner diameter is 2.3 cm, high 1 cm, wide 1.2 cm in ground shirt rim;Upper lid cavity ground shirt rim
Wide 1.2 cm, cavity internal diameter 2.3 cm, high 7 cm, air setting bore 0.5 cm, total length 30 cm, wherein 120 degree angles
Extend 10 cm vertically downward after extending 20 cm.
Described glass base is used for placing elemental selenium to be measured and heats on hot plate.
Embodiment
Instrument and reagent
UV2550 ultraviolet spectrophotometer(Japanese Shimadzu Corporation), C20L-NL909T electromagnetic oven(The limited public affairs of woods photoelectron
Department), WG1000 pure water meter(Japanese Yamato company).Selenium powder(Article No. s105194-25g, purity >=99.99%, Lycoperdon polymorphum Vitt, fusing point
For 217-222 DEG C)Come from aladdin company.Sodium sulfide is that analysis is pure, is produced by Chemical Reagent Co., Ltd., Sinopharm Group.
The drafting of standard curve
Accurately weigh elemental selenium standard substance 39.48 mg, be dissolved in 5 mL Na2S(1M)In, this is selenium standard working solution(Se
Content:100 umol/mL).
The drafting of standard curve:Accurately measure respectively 0.0,20.0,40.0,80.0,120.0,160.0,200.0 and
300.0 uL selenium standard working solution.Be equivalent to 0.0 μm of ol, 2.0 μm of ol, 4.0 μm of ol, 8.0 μm of ol, 12.0 μm of ol, 16.0
μm ol, 20.0 μm of ol and 30.0 μm of ol elemental selenium, use 1M Na2S aqueous solution is diluted to 4 mL, shakes up, and places 1 hour.Afterwards
On ultraviolet spectrophotometer, with absorbing wavelength 500 nm mensuration absorbance value.
The mensure of elemental selenium
Process selenium powder with carbonizing plant, to investigate the response rate that this device is enriched with elemental selenium.Weigh 25 mg selenium powders, be placed in
In the glass of device pedestal, cover lid cavity, upper and lower two ground positions are fitted like a glove placement, and symmetrical with fish tail folder
Fixing;Said apparatus are placed in the heating plate of electromagnetic oven, 300 DEG C of heating 30 min;1M Na is used after cooling2S aqueous solution is by cavity
It is transferred to volumetric flask including the selenium powder condensing tube portion is lossless, and use Na2S aqueous solution is settled to 25 mL.1 is taken from volumetric flask
The Na of mL selenium2S aqueous solution, adds 3 mL Na2S aqueous solution, places 1 hour, with ultraviolet spectrophotometer, by the mark of the present embodiment
The method of the drafting part of directrix curve is detected.
Result and discussion
The drafting of standard curve
Make elemental selenium standard curve as shown in figure 3, curve regression equation be y=0.028x-0.025, correlation coefficient
Square for 0.998,0 ~ 30.0 umol selenium in every 4 mL 1M Na2In S aqueous solution, concentration and absorbance are in good linear pass
System.
The mensure of elemental selenium
Measure the Na of selenium powder2S aqueous solution absorbance, calculates Se content result as shown in table 1 by standard curve, elemental selenium
The response rate be:94.06 ~ 105.27, response rate relative standard deviation is 4.55%.
Present invention could apply to elemental selenium content detection in actual Feed Sample, and other is containing organic substance and oxidation
The elemental selenium sample of state selenium compound.To those skilled in the art, by the teachings of the present invention, obtain technical scheme and become
Shape and application etc. are also within protection scope of the present invention.
Claims (1)
1. a kind of for Quantitative detection elemental selenium separate and collect device it is characterised in that adopt borosilicate glass material
Matter, including glass base, upper lid cavity, glass base is provided with ground shirt rim, and the bottom of upper lid cavity is provided with and accordingly coincide
Ground shirt rim, the top of upper lid cavity is provided with an air set pipe, the vertical line of described air set pipe and upper lid cavity with
120 degree of angle extends after stretching out vertically downward again;
Described glass base, upper lid cavity are symmetrically fixed using fish tail folder;
Described glass base, upper lid cavity, the thickness of glass of air set pipe are 0.3 cm;
Described glass base is used for placing elemental selenium to be measured and heats on hot plate;
Described glass base inner diameter is 2.3 cm, high 1 cm, wide 1.2 cm in ground shirt rim;Upper lid cavity ground shirt rim width
1.2 cm, cavity internal diameter 2.3 cm, high 7 cm, air setting bore 0.5 cm, total length 30 cm, wherein 120 degree angles prolong
Extend 10 cm vertically downward after stretching 20 cm.
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CN1283549C (en) * | 2004-12-03 | 2006-11-08 | 昆明理工大学 | Vacuum smelting process of extracting selenium |
JP2007132790A (en) * | 2005-11-10 | 2007-05-31 | Sumitomo Metal Mining Co Ltd | Quantitative analysis method of selenium by flame atomic absorption method |
CN100411975C (en) * | 2006-09-29 | 2008-08-20 | 先导(清远)稀有金属化工有限公司 | Producing device of high-purity selenium and producing process |
CN102674268A (en) * | 2011-03-11 | 2012-09-19 | 大连立方化学技术有限公司 | Hydrogen selenide preparation device and method |
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