CN105241739A - Microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber - Google Patents
Microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber Download PDFInfo
- Publication number
- CN105241739A CN105241739A CN201510712359.6A CN201510712359A CN105241739A CN 105241739 A CN105241739 A CN 105241739A CN 201510712359 A CN201510712359 A CN 201510712359A CN 105241739 A CN105241739 A CN 105241739A
- Authority
- CN
- China
- Prior art keywords
- concentration
- standard solution
- acid
- sample
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber. The method is as below: digesting a sample with nitric acid in a microwave digestion instrument; then dissolving salts in the digestion solution by using mixed acid of sulfuric acid and phosphoric acid; stabilizing the acidity of the sample solution and the standard solution; adjusting the content of matrix to match; and finally preparing a standard solution curve, and choosing a suitable analytical line for measurement in an inductively coupled high frequency plasma atomic emission spectrometer. The invention uses nitric acid for digestion of the sample, so as to replace sample dissolution in mixed acid of nitric acid and hydrofluoric acid in a common ICP-AES method for determination of high temperature alloy; the method avoids corrosion of a quartz sampling system of the inductively coupled high frequency plasma atomic emission spectrometer by hydrofluoric acid, pollution to the instrument, and factors affecting measurement accuracy. At the same time, the invention employs mixed acid of sulfuric acid and phosphoric acid to dissolve salts in the digestion solution, so as to prevent wounding by solution spill and unfavorable factors of deviation measurement.
Description
Technical field
The present invention relates to a kind of method measuring Determination of multiple metal elements content in synthetic rubber, particularly relate to the method for multielement content in a kind of microwave clearing ICP method Simultaneously test synthetic rubber.
Background technology
Aeronautics and Astronautics synthetic rubber according to needed for add appropriate metallic compound and synthesize, to meet, it is fire-retardant, heatproof, cold-resistant etc. performance, and the therefore content of the various metallic element of Measurement accuracy is the key of development and production control.At present, be generally adopt aluminium, magnesium in burning-ashing-alkali fusion-EDTA volumetric determination synthetic rubber; Employing subtracts impurity method and measures antimony; Adopt Spectrophotometric Determination of Copper, manganese.But, adopt burning-ashing-alkali fusion to prepare solution step complexity, Production Time long, easily cause sample loss, cause testing result on the low side; Adopt EDTA volumetric determination aluminium, magnesium process time long, and detect lower limit for height, low content aluminium, magnesium can not be measured; And adopt subtract impurity method measure antimony time, antimony content need detect that other all impurity just can draw; Spectrophotometric method can not measure copper, the Fe content of trace.Therefore, a kind of method of aluminium, magnesium, antimony, copper and manganese element in energy Simultaneously test Aeronautics and Astronautics synthetic rubber is not seen in prior art.
In detection alloying element means, since inductively coupled plasma (ICP) emission spectrometer came out from 1975, the advantages such as the mutual interference just because its detectability is low, precision is high, between wide, the sample composition of the mensuration range of linearity of concentration is little, become a kind of analysis means that other analytical technology is incomparable in micro-Simultaneously test.But, in traditional micro-wave digestion synthetic rubber method, normal employing nitric acid, hydrofluorite mixed-acid dissolution sample, hydrofluorite has corrosive attack to indutively coupled plasma Atomic Emission Spectrometer AES quartz sample system, easily instrument is polluted, the accuracy that impact measures and repeatability, and adopt the wayward sample solution of nitric acid and standard solution acidity separately, easily cause solution acidity inconsistent, affect measurement result.
Summary of the invention
The object of the invention is to: provide a kind of method fast, accurately, to multielement content in instrument free of contamination microwave clearing ICP method Simultaneously test synthetic rubber, to overcome the deficiencies in the prior art.
Technical scheme of the present invention: a kind of method of multielement content in microwave clearing ICP method Simultaneously test synthetic rubber, comprises the following steps:
A, take synthetic rubber sample 0.1g and be placed in micro-wave diminishing pot, then add the nitric acid 5mL ~ 7mL of 1.42g/mL, the counteracting tank that sample is housed also, after tightening, is put into microwave dissolver by cover lid;
B, startup microwave dissolver, carry out intermittent type microwave by following micro-wave digestion program and clear up: (1) power 900W, heating schedule are be incubated 20 minutes after within 5 minutes, being warming up to 150 DEG C; (2) power 900W, heating schedule are be incubated 15 minutes after within 1 minute, being warming up to 150 DEG C; (3) power 900W, heating schedule are be incubated 30 minutes after within 1 minute, being warming up to 200 DEG C; (4) power 900W, heating schedule are be incubated 30 minutes after within 1 minute, being cooled to 100 DEG C; (5) finally under the condition of 50 DEG C, be incubated 10 minutes, complete micro-wave digestion program; After clearing up EOP (end of program), digester is put into chilled water and is chilled to room temperature;
C, said sample solution is transferred in 150mL beaker, add the acid mixture that sulfuric acid 10mL that concentration is 1.84g/mL and concentration are the phosphoric acid 5mL of 1.70g/mL, then beaker is placed on electric hot plate and is heated to just smolder, drip the nitric acid 5mL that concentration is 1.42g/mL, continue to be heated to solution limpid and smolder, take off and be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, mixing;
D, draw copper that concentration is the aluminium of 10mg/mL, each 10mL of magnesium standard solution, concentration are 1mg/mL antimony standard solution 10mL and concentration are 1g/mL, each 1.0mL of manganese standard solution in the volumetric flask of 100mL respectively, mix after being diluted with water to scale, obtained mixed standard solution;
E, pipette mixed standard solution 0mL respectively, 1.0mL, 5.0mL, 10.0mL is in the volumetric flask of 4 100mL, respectively add the acid mixture that sulfuric acid 10mL that concentration is 1.84g/mL and concentration are the phosphoric acid 5mL of 1.70g/mL, then beaker is placed on electric hot plate and is heated to just smolder, drip the nitric acid 5mL that concentration is 1.42g/mL, continue to be heated to solution limpid and smolder, take off and be cooled to room temperature, move in 100mL volumetric flask, make acidity in each volumetric flask consistent, to be made into calibration curve series standard solution after water constant volume respectively, then according to the condition of work of ICP spectrometer, above-mentioned standard solution is measured, with each element massfraction to be measured for horizontal ordinate, emissive porwer is ordinate, by computer drawing calibration curve, just each constituent content can be calculated by calibration curve.
In said method, the every 1mL of the mixed standard solution described in steps d contains aluminium, each 1mg of magnesium respectively, containing antimony 100 μ g, and cupric, each 10 μ g of manganese respectively.
In said method, in the series standard solution described in step e, the concentration of aluminium, magnesium is equivalent to the massfraction sum of aluminium in sample, magnesium, is respectively 0.0%, 1.00%, 5.00%, 10.00%; In series standard solution, the concentration of antimony is equivalent to the massfraction of antimony in sample, is respectively 0.0%, 0.10%, 0.50%, 1.00%; In series standard solution, the concentration of copper, manganese is equivalent to the massfraction sum of copper in sample, manganese, is respectively 0.0%, 0.01%, 0.050%, 0.10%.
Compared with prior art, the invention has the advantages that: the present invention adopts nitric acid to clear up test portion, instead of the mixed-acid dissolution sample that general ICP-AES measures nitric acid, hydrofluorite in high temperature alloy method, hydrofluorite is avoided to corrode the quartz sample system of indutively coupled plasma Atomic Emission Spectrometer AES, instrument is polluted, affects the factor of measurement accuracy.Meanwhile, the present invention adopts the salt in the mixed-acid dissolution digestion solution of sulfuric acid, phosphoric acid, prevents solution to spill to hurt sb.'s feelings and cause the unfavorable factor of measured deviation.In addition, because method of the present invention can multielement content in Simultaneously test synthetic rubber, thus overcome and adopt burning-ashing-alkali fusion to prepare use EDTA volumetric method, spectrophotometric method after solution, subtract impurity method to measure Al, Mg, Sb, Cu, Mn element respectively and cause complicated operation, Production Time long, easily cause sample loss, cause the problem of testing result deviation.Be proven, method of the present invention is adopted to measure the massfraction of aluminium, magnesium in the method for metal multielement content in synthetic rubber in 1.00% ~ 10.00% scope, the massfraction of antimony is in 0.10% ~ 1.00% scope, the massfraction of copper, manganese is in 0.010% ~ 0.10% scope, the RSD of each element determination result is all less than 5%, precision is better, accuracy in detection is high, for the production control of Aeronautics and Astronautics synthetic rubber, scientific research provide metal multielement compositional data accurately, guarantee space flight, aeronautical product quality.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearly, below in conjunction with embodiment, the present invention is described in further detail.
Embodiment
A kind of microwave clearing ICP method of the present invention measures the method for indissoluble nickel base superalloy multielement content, comprises the following steps:
A, take synthetic rubber sample 0.1g and be placed in micro-wave diminishing pot, then add the nitric acid 5mL ~ 7mL of 1.42g/mL, the counteracting tank that sample is housed also, after tightening, is put into microwave dissolver by cover lid;
B, startup microwave dissolver, carry out intermittent type microwave by following micro-wave digestion program and clear up:
That is: (1) power 900W, heating schedule are be incubated 20 minutes after within 5 minutes, being warming up to 150 DEG C; (2) power 900W, heating schedule are be incubated 15 minutes after within 1 minute, being warming up to 150 DEG C; (3) power 900W, heating schedule are be incubated 30 minutes after within 1 minute, being warming up to 200 DEG C; (4) power 900W, heating schedule are be incubated 30 minutes after within 1 minute, being cooled to 100 DEG C; (5) finally under the condition of 50 DEG C, be incubated 10 minutes, complete micro-wave digestion program; After clearing up EOP (end of program), digester is put into chilled water and is chilled to room temperature;
C, said sample solution is transferred in 150mL beaker, add the acid mixture that sulfuric acid 10mL that concentration is 1.84g/mL and concentration are the phosphoric acid 5mL of 1.70g/mL, then beaker is placed on electric hot plate and is heated to just smolder, drip the nitric acid 5mL that concentration is 1.42g/mL, continue to be heated to solution limpid and smolder, take off and be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, mixing;
D, draw copper that concentration is the aluminium of 10mg/mL, each 10mL of magnesium standard solution, concentration are 1mg/mL antimony standard solution 10mL and concentration are 1g/mL, each 1.0mL of manganese standard solution in the volumetric flask of 100mL respectively, mix after being diluted with water to scale, obtained mixed standard solution; The every 1mL of described mixed standard solution contains aluminium, each 1mg of magnesium respectively, containing antimony 100 μ g, and cupric, each 10 μ g of manganese respectively.
E, pipette mixed standard solution 0mL, 1.0mL, 5.0mL, 10.0mL in the volumetric flask of 4 100mL respectively, respectively add the acid mixture that sulfuric acid 10mL that concentration is 1.84g/mL and concentration are the phosphoric acid 5mL of 1.70g/mL, then beaker is placed on electric hot plate and is heated to just smolder, drip the nitric acid 5mL that concentration is 1.42g/mL, continue to be heated to solution limpid and smolder, take off and be cooled to room temperature, move in 100mL volumetric flask, make acidity in each volumetric flask consistent, to be made into calibration curve series standard solution after water constant volume respectively; In described series standard solution, the concentration of aluminium, magnesium is equivalent to the massfraction sum of aluminium in sample, magnesium, is respectively 0.0%, 1.00%, 5.00%, 10.00%; In series standard solution, the concentration of antimony is equivalent to the massfraction of antimony in sample, is respectively 0.0%, 0.10%, 0.50%, 1.00%; In series standard solution, the concentration of copper, manganese is equivalent to the massfraction sum of copper in sample, manganese, is respectively 0.0%, 0.01%, 0.050%, 0.10%.Now, measure above-mentioned standard solution according to the condition of work of ICP spectrometer, with each element massfraction to be measured for horizontal ordinate, emissive porwer is ordinate, by computer drawing calibration curve, just can calculate each constituent content by calibration curve.
Be proven, method of the present invention is adopted to measure the massfraction of aluminium, magnesium in the method for metal multielement content in synthetic rubber in 1.00% ~ 10.00% scope, the massfraction of antimony is in 0.10% ~ 1.00% scope, the massfraction of copper, manganese is in 0.010% ~ 0.10% scope, the RSD of each element determination result is all less than 5%, precision is better, accuracy in detection is high, for the production control of Aeronautics and Astronautics synthetic rubber, scientific research provide metal multielement compositional data accurately, guarantee space flight, aeronautical product quality.
Claims (3)
1. the method for multielement content in microwave clearing ICP method Simultaneously test synthetic rubber, is characterized in that comprising the following steps:
A, take synthetic rubber sample 0.1g and be placed in micro-wave diminishing pot, then add the nitric acid 5mL ~ 7mL of 1.42g/mL, the counteracting tank that sample is housed also, after tightening, is put into microwave dissolver by cover lid;
B, startup microwave dissolver, carry out intermittent type microwave by following micro-wave digestion program and clear up: (1) power 900W, heating schedule are be incubated 20 minutes after within 5 minutes, being warming up to 150 DEG C; (2) power 900W, heating schedule are be incubated 15 minutes after within 1 minute, being warming up to 150 DEG C; (3) power 900W, heating schedule are be incubated 30 minutes after within 1 minute, being warming up to 200 DEG C; (4) power 900W, heating schedule are be incubated 30 minutes after within 1 minute, being cooled to 100 DEG C; (5) finally under the condition of 50 DEG C, be incubated 10 minutes, complete micro-wave digestion program; After clearing up EOP (end of program), digester is put into chilled water and is chilled to room temperature;
C, said sample solution is transferred in 150mL beaker, add the acid mixture that sulfuric acid 10mL that concentration is 1.84g/mL and concentration are the phosphoric acid 5mL of 1.70g/mL, then beaker is placed on electric hot plate and is heated to just smolder, drip the nitric acid 5mL that concentration is 1.42g/mL, continue to be heated to solution limpid and smolder, take off and be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, mixing;
D, draw copper that concentration is the aluminium of 10mg/mL, each 10mL of magnesium standard solution, concentration are 1mg/mL antimony standard solution 10mL and concentration are 1g/mL, each 1.0mL of manganese standard solution in the volumetric flask of 100mL respectively, mix after being diluted with water to scale, obtained mixed standard solution;
E, pipette mixed standard solution 0mL respectively, 1.0mL, 5.0mL, 10.0mL is in the volumetric flask of 4 100mL, respectively add the acid mixture that sulfuric acid 10mL that concentration is 1.84g/mL and concentration are the phosphoric acid 5mL of 1.70g/mL, then beaker is placed on electric hot plate and is heated to just smolder, drip the nitric acid 5mL that concentration is 1.42g/mL, continue to be heated to solution limpid and smolder, take off and be cooled to room temperature, move in 100mL volumetric flask, make acidity in each volumetric flask consistent, to be made into calibration curve series standard solution after water constant volume respectively, then according to the condition of work of ICP spectrometer, above-mentioned standard solution is measured, with each element massfraction to be measured for horizontal ordinate, emissive porwer is ordinate, by computer drawing calibration curve, just each constituent content can be calculated by calibration curve.
2. the method for multielement content in microwave clearing ICP method Simultaneously test synthetic rubber according to claim 1, is characterized in that: the every 1mL of the mixed standard solution described in steps d respectively containing aluminium, each 1mg of magnesium, containing antimony 100 μ g, cupric, each 10 μ g of manganese respectively.
3. the method for multielement content in microwave clearing ICP method Simultaneously test synthetic rubber according to claim 1, it is characterized in that: in the series standard solution described in step e, the concentration of aluminium, magnesium is equivalent to the massfraction sum of aluminium in sample, magnesium, is respectively 0.0%, 1.00%, 5.00%, 10.00%; In series standard solution, the concentration of antimony is equivalent to the massfraction of antimony in sample, is respectively 0.0%, 0.10%, 0.50%, 1.00%; In series standard solution, the concentration of copper, manganese is equivalent to the massfraction sum of copper in sample, manganese, is respectively 0.0%, 0.01%, 0.050%, 0.10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510712359.6A CN105241739A (en) | 2015-10-28 | 2015-10-28 | Microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510712359.6A CN105241739A (en) | 2015-10-28 | 2015-10-28 | Microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105241739A true CN105241739A (en) | 2016-01-13 |
Family
ID=55039462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510712359.6A Pending CN105241739A (en) | 2015-10-28 | 2015-10-28 | Microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105241739A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105928925A (en) * | 2016-07-12 | 2016-09-07 | 广西壮族自治区分析测试研究中心 | ICP-AES method for determining sulphur content in lead sulfate desulfurized product of waste battery |
| CN105954262A (en) * | 2016-07-12 | 2016-09-21 | 广西壮族自治区分析测试研究中心 | {0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery |
| CN107589108A (en) * | 2017-10-27 | 2018-01-16 | 贵州航天精工制造有限公司 | A kind of method of metal oxide content in measure rubber |
| CN109406495A (en) * | 2018-11-06 | 2019-03-01 | 郑州翱翔医药科技股份有限公司 | It can extract the detection method of metal ion in a kind of rubber piston |
| CN113340977A (en) * | 2021-06-09 | 2021-09-03 | 苏州微敏检测技术服务有限公司 | Method for measuring content of sulfur element in rubber plug extracting solution by ICP-MS (inductively coupled plasma-Mass Spectrometry) |
| CN116642876A (en) * | 2023-05-05 | 2023-08-25 | 北京先通国际医药科技股份有限公司 | Method for determining content of related metal elements in yttrium-containing glass microspheres and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590183A (en) * | 2012-03-06 | 2012-07-18 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method capable of quantitatively screening substance of very high concern in rubber and plastic products using microwave digestion-ICP-AES method |
-
2015
- 2015-10-28 CN CN201510712359.6A patent/CN105241739A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590183A (en) * | 2012-03-06 | 2012-07-18 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method capable of quantitatively screening substance of very high concern in rubber and plastic products using microwave digestion-ICP-AES method |
Non-Patent Citations (6)
| Title |
|---|
| 丁晓英等: "橡胶制品化学测试方法国际标准现状及进展", 《广州化工》 * |
| 无: "微波消解轮胎橡胶", 《百度文库》 * |
| 机械工业理化检验人员技术培训和资格鉴定委员会等: "《金属材料化学分析》", 30 June 2015, 科学普及出版社 * |
| 王守宇等: "丁苯类橡胶鞋底微波消解方法的研究", 《中国皮革》 * |
| 邓江华等: "电感耦合等离子体原子发射光谱法测定橡胶中微量元素", 《理化检验-化学分册》 * |
| 郑向前等: "微波消解-紫外分光光度法测定天然橡胶中锰含量", 《热带作物学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105928925A (en) * | 2016-07-12 | 2016-09-07 | 广西壮族自治区分析测试研究中心 | ICP-AES method for determining sulphur content in lead sulfate desulfurized product of waste battery |
| CN105954262A (en) * | 2016-07-12 | 2016-09-21 | 广西壮族自治区分析测试研究中心 | {0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery |
| CN107589108A (en) * | 2017-10-27 | 2018-01-16 | 贵州航天精工制造有限公司 | A kind of method of metal oxide content in measure rubber |
| CN109406495A (en) * | 2018-11-06 | 2019-03-01 | 郑州翱翔医药科技股份有限公司 | It can extract the detection method of metal ion in a kind of rubber piston |
| CN113340977A (en) * | 2021-06-09 | 2021-09-03 | 苏州微敏检测技术服务有限公司 | Method for measuring content of sulfur element in rubber plug extracting solution by ICP-MS (inductively coupled plasma-Mass Spectrometry) |
| CN116642876A (en) * | 2023-05-05 | 2023-08-25 | 北京先通国际医药科技股份有限公司 | Method for determining content of related metal elements in yttrium-containing glass microspheres and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105241739A (en) | Microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber | |
| CN105319202A (en) | Method for measuring indissolvable nickel-base superalloy multielement content with microwave digestion ICP method | |
| CN101718689B (en) | Method for measuring contents of aluminum, titanium, manganese, nickel, tungsten and iron in cobalt-base alloy | |
| CN101644677B (en) | Method for detecting element content in alloy or ore by utilizing ICP emission spectrometer | |
| CN103267754B (en) | The method of macroelement and arsenic, tin, antimony trace element in quantitative measurement carbon steel or low alloy steel | |
| CN108982204A (en) | A kind of method that micro-wave digestion-ICP-OES measures microelement in graphite | |
| CN107576680B (en) | Method for analyzing niobium-tantalum ore by low dilution ratio melting X-ray fluorescence spectrum | |
| CN102735678A (en) | Method for determining chromium content and aluminum content in nickel-chromium-aluminum coated diatomite | |
| CN103454131B (en) | The efficient assay method of cobalt, nickel, aluminium content in a kind of natural micro alloy iron powder | |
| CN102213657A (en) | Digestion method and detection method of Tungsten-base class sample | |
| CN102565026A (en) | Method for measuring silicon content in aluminum manganese iron | |
| CN104807813A (en) | Rapid analysis method for content of manganese in ferromanganese iron | |
| CN105136777A (en) | Method for measuring trace element content in aluminium alloy by ICP method | |
| CN103674932A (en) | Method for determining content of Cu, Mn and Sn in Cu-Mn-Sn alloyed powder through ICP (inductively coupled plasma) | |
| CN108872203A (en) | The detection method of elemental composition in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag | |
| CN104316590A (en) | Inductively coupled plasma mass spectrometry method for simultaneous determination of chromium, nickel, arsenic and lead in hot melt adhesive for cigarette | |
| CN105203698A (en) | Method for directly determining aluminum content in aluminum-niobium alloy | |
| CN104089947A (en) | Method for detecting chemical components comprising nickel, chromium and manganese of stainless steel | |
| CN103940650B (en) | A kind of measure the method for ferrum nickel in high density tungsten basigamy pouring weight | |
| CN112763481B (en) | Method for measuring trace selenium, cerium, zirconium, tantalum and tellurium content in nickel-based alloy by ICP-MS method | |
| CN105806826A (en) | Method for determining content of elements in potassium-bearing ore by ICP (Inductively Coupled Plasma) internal standard method | |
| CN104034573B (en) | A kind of digestion procedure of nickel-base alloy | |
| CN103954610A (en) | Method for measuring arsenic in high-chromium high-nickel steel | |
| CN105784677A (en) | Method for determination of impurity elements in boron carbide alumina core block | |
| CN110412201A (en) | A kind of method of lithium, sodium, potassium, rubidium, caesium in measurement lithium ore |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160113 |