CN101688823B - 用于定量和定性确定钾和镁矿石的加工产品中的贵金属含量的样品的制备方法 - Google Patents
用于定量和定性确定钾和镁矿石的加工产品中的贵金属含量的样品的制备方法 Download PDFInfo
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- 239000011591 potassium Substances 0.000 title claims description 4
- 229910052700 potassium Inorganic materials 0.000 title claims description 4
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- 235000002639 sodium chloride Nutrition 0.000 abstract description 14
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- 239000010931 gold Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000011435 rock Substances 0.000 description 9
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- 150000003839 salts Chemical class 0.000 description 5
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- 238000007796 conventional method Methods 0.000 description 3
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
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- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 238000009828 non-uniform distribution Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Manufacture And Refinement Of Metals (AREA)
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Abstract
本发明涉及用于钾加工工厂的粘土盐废料(浆料)的分析化学和加工技术。本发明的方法基于测试材料总体的分析并包括在氯化钾(KCl)或氯化钠(NaCl)形式的氯化物试剂的存在下在600至950℃的温度下将贵金属(Au、Pt、Pd)有机化合物的纳米粒子退火，并包括制备所述金属的酸可溶性化合物。将所述样品暴露于整个技术转化循环：1)氯化焙烧；2)用弱无机酸溶液溶滤；3)在溶滤之后将贵金属化合物从所得溶液吸附至工业吸附剂AM-2B 4上，以及4)解吸。分析在所述循环结束时获得的可销售的溶液的贵金属含量。与用于常规分析方法的3-30克的非代表性的测试部分不同，所述发明有可能使用给定测试阶段所需的测试部分，并排除分析中测试材料的“遗漏”。
Description
本发明涉及钾生产工厂的粘土盐(argillo-saline)废料(浆料)的分析化学和加工技术的领域，并可应用于自浆料的水不可溶残余物、含盐岩石和它们的加工产物回收的贵金属(Au、Pt、Pd)含量的定量和定性测定。
存在由Central Laboratory for Substance Analysis of the VernadskyInstitute of Geochemistry&Analytical Chemistry(ЦЛAB ΓEOXИ)设计的一些已知方法，如“Precious Metals.Determination of Their Content inNatural Subjects by Method of Electrothermic Atomic Absorption(EAA)”(出版于1997年)和“Precious Metals. Determination of Their Content byMethod of Atomic Emission with the Use of Plasma Fixed by Inducti
为了进行分析，必须将在先称重的1克样品置入钛高压釜的氟塑料套管[杯](150毫升)中并将4毫升硝酸(HNO3)+4毫升盐酸(HCl)+4毫升过氧化氢(H2O2)倒入样品。在220℃下静置该混合物4小时。然后将所述套管[杯]中的内容物转移至玻璃碳杯中，加入15毫升氢氟酸(HF)，将该混合物放置在电热板(炉)上并蒸发至干。为了去除氟蒸汽，加入5毫升盐酸(HCl)，将该混合物蒸发至干并混入15毫升王水(以1HNO3比3HCl的比例)。将该混合物蒸发至湿[潮湿]的盐，加入5毫升盐酸(HCl)并再次蒸发至湿[潮湿]的盐以去除所有的二氧化氮(NO2)蒸汽。使用二当量(binormal)盐酸(2N HCl)将内容物转移至溶液。下一步为提取(甲基异丁酮)以测定金(Au)含量或者为吸附(Polyorgs-IV吸附剂)以测定铂(Pt)和钯(Pd)含量。
考虑到贵金属化合物是不均匀地分布于水不可溶浆料中或者含盐岩石和(或)它们的加工产品中，这些方法的弱点为与小的被分析重量相关的结果的不可靠性。电子(technotronic)有机物质的存在对非均匀分布具有另外的作用。
由专利涵盖的本发明有助于解决高度可靠结果的问题。
在Verkhnekamskoje田地(field)的含盐岩石中存在的贵金属以掺入含盐岩石的水不可溶残余物中，且在矿石加工的情况中为掺入粘土盐废料(浆料)的水不可溶残余物中的Au、Pt和Pd的有机化合物为代表。
测定对照岩石中的贵金属含量，其水不可溶残余物和浆料的水不可溶残余物造成严重的问题。问题是当水不可溶残余物自盐(盐水(saline))基体分离时，其有机组分的结构和组成被改性，这显示为Au、Pt和Pd的有机化合物的结块(blocking)、它们的聚集、含盐岩石或浆料的水不可溶残余物中的组成和重排(rearrangement)的改变。电子有机物质(胺和聚丙烯酰胺)的存在加快并增强了该过程。结果，含盐岩石和它们的加工产品的水不可溶残余物中的贵金属的抽样法和正确分析(化验)不会正确地进行。发展浆料加工的工业技术以回收贵金属的主要挑战是确定对照原料(浆料)、中间产物(炉渣、滤饼、生产溶液)和主要产物(市售溶液)中的贵金属(Au、Pt、Pd)含量。该问题特别困难。
首先，必须开发结块化合物的分解方法，第二，必须消除可与贵金属一起分解的附带元素的影响。比如，将炉渣溶滤(leached)时获得的溶液(下文称作生产溶液)含有相当大量的附带金属，例如亲硫元素(Co、Ni、Cu、Zn、As、Pb、Sb、Bi)的含量(根据对照原料)为0.5克/吨或0.5克/吨以上；锌的含量为370克/吨之多，稀土元素(14种元素)的含量为至少0.66克/吨。铈、稀有金属、碱土元素、铀(U)和钍(Th)的含量分别为32克/吨、3克/吨、100克/吨、5克/吨和6克/吨。通过ISP和EAA法对生产溶液的分析给出前者的质谱叠加和后者的合法[有效]信号抑制。因此，贵金属(Au、Pt、Pd)的含量显得被低估。
在另一方面，贵金属(Au、Pt、Pd)化合物的重排和它们的聚集可造成在待分析的3-30克称重样品[在先称重的样品]中不存在这种化合物，即称重样品[样品]根本不是代表性的。
基于被分析材料的特定特征，开发了作为“技术分析”的概念[想法]结合的整个技术系统。该系统的基本构成为用于分析的样品的制备方法。其与常规方法的基本差异不在于将样品完全分解至溶液，而在于使用氯化焙烧自称重样品[在先称重样品]选择性回收贵金属化合物(Au、Pt、Pd)以及通过随后经由这些金属的吸附和解吸将它们溶滤至溶液从而将它们转化为酸可溶形式。解吸产物通过常规方法进行分析(EAA、AES-ISP等)。
为了获得含盐岩石和它们的加工产品的不可溶残余物的样品的制备(以用于贵金属含量的质量和数量，包括焙烧)的上述技术结果，被分析材料的称重样品[在先称重样品]的吸附和解吸的区别在于精确称重以制备市售溶液，该市售溶液的任何部分均代表被分析材料的整个样品。使称重样品在600-950℃的温度下经受氯化焙烧，在此后可能进行焙烧所形成的贵金属的酸可溶性化合物的选择性溶解、贵金属化合物溶液的吸附和解吸。
使该方法区别于类似方法的主要特征在于精确称重以制备市售溶液，该市售溶液的任何部分均代表被分析材料的整个样品。使称重样品在600-950℃的温度下经受氯化焙烧，在此后可能进行焙烧所形成的贵金属的酸可溶性化合物的选择性溶解、贵金属化合物溶液的吸附和解吸。
根据该方法，将所有量的材料进行分析，在分析过程中在可为氯化钾(KCl)和氯化钠(NaCl)的氯化物试剂的存在下在600-950℃的温度下通过氯化焙烧将贵金属(Au、Pt和Pd)的有机化合物的纳米粒子焙烧，当被分析的称重样品[在先称重样品]完全转移至溶液中时，所述形式的金属为可用无机酸溶液溶滤(区别于常规方法)的酸可溶性化合物，也就是说，发生贵金属的选择性溶解。样品经受技术转化的全部循环：1)氯化焙烧；2)用无机酸的弱溶液溶滤；3)自所得贵金属化合物的溶液吸附至吸附剂AM-2B(OST 95.291-86-Weakly BasicAnion- Exchange Resin Obtained through Successive Reactions ofChloromethylation and Amylation with Dimethyl
为了说明，我们取用10千克水不可溶残余物，加入10-25％的氯化钾(KCl)和氯化钠(NaCl)并搅拌。然后我们在马弗炉中在600-950℃的温度下进行氯化焙烧。之后，我们使“炉渣”冷却、将其研磨(将其微细分割)并置入反应容器以在搅拌下进行通过在氯化钾(KCl)和氯化钠(NaCl)的存在下在盐酸中焙烧Au、Pt和Pd的有机化合物所形成的贵金属(Au、Pt、Pd)的酸可溶性化合物的选择性溶解3-4小时。然后我们过滤矿浆，将滤液转移(泵送)至帕丘卡(Pachuca)反应器，装入吸附剂并利用空气喷嘴进行吸附搅拌。然后我们进行吸附剂洗涤并解吸。解吸的结果为市售溶液并代表被分析的样品。该溶液的任何部分均代表整个样品。
因此，基于所述结果，我们可断定已改变了含盐岩石和它们的加工产品中贵金属(Au、Pt、Pd)含量的确定的方法。
Claims (1)
1.用于定量和定性确定钾和镁矿石的加工产品中的贵金属含量的样品的制备方法，其包括被分析材料的在先称重样品的焙烧、吸附和解吸，其特征在于，称重样品以制备任何部分均代表被分析材料的整个样品的市售溶液，随即将该称重样品与以称重样品的10至25％的量加入的Na和K的氯化物混合，该称重样品进一步在600至950℃的温度下经受氯化焙烧，随即进行在焙烧称重样品上形成的酸可溶性贵金属化合物的选择性溶解，然后进行所得贵金属化合物溶液的吸附和它们随后的解吸。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2007128507/28A RU2347206C1 (ru) | 2007-07-24 | 2007-07-24 | Способ подготовки проб нерастворимого остатка соляных пород и продуктов их переработки для качественного и количественного определения содержания благородных металлов |
| RU2007128507 | 2007-07-24 | ||
| PCT/RU2008/000436 WO2009014473A1 (ru) | 2007-07-24 | 2008-07-03 | Способ подготовки проб для качественного и количественного определения содержания благородных металлов в продуктах переработки калийномагниевых руд |
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|---|---|
| CN101688823A CN101688823A (zh) | 2010-03-31 |
| CN101688823B true CN101688823B (zh) | 2011-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008800241320A Expired - Fee Related CN101688823B (zh) | 2007-07-24 | 2008-07-03 | 用于定量和定性确定钾和镁矿石的加工产品中的贵金属含量的样品的制备方法 |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US20100202944A1 (zh) |
| EP (1) | EP2169378A1 (zh) |
| CN (1) | CN101688823B (zh) |
| BR (1) | BRPI0814779A2 (zh) |
| CA (1) | CA2693950A1 (zh) |
| IL (1) | IL202777A0 (zh) |
| RU (1) | RU2347206C1 (zh) |
| WO (1) | WO2009014473A1 (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675513A (zh) * | 2016-01-18 | 2016-06-15 | 西宁特殊钢股份有限公司 | 一种电渣重熔金属熔池形貌的测定方法 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3056294B1 (fr) * | 2016-09-20 | 2020-02-14 | Kabcyt | Dispositif de capture de particules biologiques |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN88100968A (zh) * | 1988-02-25 | 1988-10-12 | 刘福喜 | 粉末标液渗凝法配制岩矿金测试标样 |
| SU1518792A1 (ru) * | 1987-08-14 | 1989-10-30 | Красноярский Филиал Всесоюзного Научно-Исследовательского И Конструкторского Института "Цветметавтоматика" | Способ разложени золотосодержащих проб |
| SU1608515A1 (ru) * | 1989-01-13 | 1990-11-23 | Государственный научно-исследовательский и проектно-конструкторский институт гидрометаллургии цветных металлов "Гидроцветмет" | Способ подготовки проб платино-содержащих материалов дл атомно-спектрального анализа |
| CN1249425A (zh) * | 1999-08-20 | 2000-04-05 | 北京矿冶研究总院 | 用于x射线光谱分析的制样方法 |
| RU2235140C2 (ru) * | 2002-12-06 | 2004-08-27 | Горный институт Уральского отделения РАН | Способ извлечения благородных металлов |
| RU2291907C1 (ru) * | 2006-01-10 | 2007-01-20 | Закрытое Акционерное Общество "Уралкалий-Технология" | Способ извлечения благородных металлов |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7067090B2 (en) * | 2002-10-25 | 2006-06-27 | South Dakota School Of Mines And Technology | Recovery of platinum group metals |
-
2007
- 2007-07-24 RU RU2007128507/28A patent/RU2347206C1/ru not_active IP Right Cessation
-
2008
- 2008-07-03 EP EP08794053A patent/EP2169378A1/en not_active Withdrawn
- 2008-07-03 WO PCT/RU2008/000436 patent/WO2009014473A1/ru active Application Filing
- 2008-07-03 BR BRPI0814779-5A2A patent/BRPI0814779A2/pt not_active IP Right Cessation
- 2008-07-03 CA CA2693950A patent/CA2693950A1/en not_active Abandoned
- 2008-07-03 CN CN2008800241320A patent/CN101688823B/zh not_active Expired - Fee Related
- 2008-07-03 US US12/452,261 patent/US20100202944A1/en not_active Abandoned
-
2009
- 2009-12-16 IL IL202777A patent/IL202777A0/en unknown
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1518792A1 (ru) * | 1987-08-14 | 1989-10-30 | Красноярский Филиал Всесоюзного Научно-Исследовательского И Конструкторского Института "Цветметавтоматика" | Способ разложени золотосодержащих проб |
| CN88100968A (zh) * | 1988-02-25 | 1988-10-12 | 刘福喜 | 粉末标液渗凝法配制岩矿金测试标样 |
| SU1608515A1 (ru) * | 1989-01-13 | 1990-11-23 | Государственный научно-исследовательский и проектно-конструкторский институт гидрометаллургии цветных металлов "Гидроцветмет" | Способ подготовки проб платино-содержащих материалов дл атомно-спектрального анализа |
| CN1249425A (zh) * | 1999-08-20 | 2000-04-05 | 北京矿冶研究总院 | 用于x射线光谱分析的制样方法 |
| RU2235140C2 (ru) * | 2002-12-06 | 2004-08-27 | Горный институт Уральского отделения РАН | Способ извлечения благородных металлов |
| RU2291907C1 (ru) * | 2006-01-10 | 2007-01-20 | Закрытое Акционерное Общество "Уралкалий-Технология" | Способ извлечения благородных металлов |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675513A (zh) * | 2016-01-18 | 2016-06-15 | 西宁特殊钢股份有限公司 | 一种电渣重熔金属熔池形貌的测定方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2169378A1 (en) | 2010-03-31 |
| CN101688823A (zh) | 2010-03-31 |
| RU2347206C1 (ru) | 2009-02-20 |
| WO2009014473A1 (ru) | 2009-01-29 |
| BRPI0814779A2 (pt) | 2015-03-03 |
| CA2693950A1 (en) | 2009-01-29 |
| IL202777A0 (en) | 2010-06-30 |
| US20100202944A1 (en) | 2010-08-12 |
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