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CN103592197B - A heavy Selenium Selenium Content Analysis Method - Google Patents

A heavy Selenium Selenium Content Analysis Method Download PDF

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CN103592197B
CN103592197B CN 201310545957 CN201310545957A CN103592197B CN 103592197 B CN103592197 B CN 103592197B CN 201310545957 CN201310545957 CN 201310545957 CN 201310545957 A CN201310545957 A CN 201310545957A CN 103592197 B CN103592197 B CN 103592197B
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CN103592197A (en )
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梁海卫
龚昌合
朱新生
陈燕
陈丽
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铜陵有色金属集团股份有限公司
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Abstract

本发明公开了一种分析粗硒中硒含量的方法,它包括试样酸溶解,过滤,分离酸不溶元素干扰;水合肼还原,过滤,分离部分干扰元素;沉淀再经酸溶解,光谱仪测定碲,排除主要干扰元素;滤液经光谱仪测定硒含量,对分析结果进行补正。 The present invention discloses a method of analyzing the crude selenium selenium content of a sample which comprises dissolving an acid, by filtration, separating the acid-insoluble interference element; hydrazine, filtered and separated partial interference element; pellet was dissolved by the acid, tellurium spectrometer , major interfering elements excluded; selenium content in the filtrate was measured by spectrometer analysis result corrected. 方法采用经典的重量法测定,消除主要干扰元素,补正滤液硒的损失,方法结果准确可靠,分析范围广,不但可以测定粗硒,还可以测定硒含量在99.9%以下的纯硒,具有较大的推广价值。 Methods Determination of weight classical, mainly to eliminate interfering elements, selenium filtrate loss corrected, the result is accurate and reliable method, a wide range of analysis, not only coarse measurement of selenium, selenium content can also be determined pure selenium 99.9% or less, having a larger promotional value.

Description

一种分析粗硒中硒含量的方法 A heavy Selenium Selenium Content Analysis Method

技术领域 FIELD

[0001] 本发明涉及一种分析粗硒中硒含量的方法。 [0001] The present invention relates to a method of analyzing the crude selenium content of selenium.

背景技术 Background technique

[0002] 硒是一种重要的工业原料,也是动物和人体所必需的微量元素之一。 [0002] Selenium is an important industrial raw materials, is one of the trace elements necessary for animals and humans. 硒在自然界中稀少、分散,很少有集中的矿床,地壳中的含量为一亿分之一。 Selenium rare in nature, dispersed, there is little focus on deposits, the content of the earth's crust is one hundred million. 由于硒具有光敏感、半导体等特性,所以常用来制造光敏元件、光学仪器、电器元件等。 Because selenium has a light-sensitive semiconductor properties, so that the photosensitive member used to manufacture, optical instruments, electrical components and the like. 在冶金、玻璃、化学等工业领域,硒得到了广泛的应用;在营养、医学、生命科学上,它是人体重要的微量元素。 In industry metallurgy, glass, chemicals, etc., selenium has been widely used; in nutrition, medicine, life sciences, it is the body's important trace elements. 20世纪初,世界上已开始了硒的生产,但由于硒资源稀少、含量极低、提取工艺复杂、价格昂贵等诸多因素的影响,导致其工业应用受到很大的影响。 Early 20th century, the world has begun production of selenium, but selenium resources are scarce, the content is very low, the impact process is complex, expensive, and many other factors of extraction, leading to its industrial application is greatly affected. 随着科学技术的进步和世界经济的迅猛发展,尤其是当今尖端科技领域的不断拓展,硒的应用领域不断扩大,其应用主要集中在石油、化工、电子、电器、玻璃、冶金、陶瓷、医药工业等领域,并逐渐渗透到其他相关领域。 With the rapid development of scientific and technological progress and the world economy, especially in today's cutting-edge technology in the field of expanding, expanding the field of application of selenium, which is mainly applied in petroleum, chemical, electronics, electrical appliances, glass, metallurgy, ceramics, pharmaceuticals industry and other fields, and gradually penetrate into other related areas. 硒的应用已不断有新的发展,半导体制冷元件、热电材料和太阳能电池是硒当今和未来的发展方向。 Selenium applications has continued to develop new, thermoelectric cooling element, and the thermoelectric material selenium solar cell current and future development direction. 因此,硒是现代工业高度发展,尤其是未来高端科技发展不可缺少的物质。 Therefore, selenium is a highly modern industrial development, especially the development of future high-end technology indispensable material.

[0003] 提取硒的主要原料为有色金属电解产出的阳极泥,其中居于首位的是铜电解的阳极泥,其次是镍和铅电解的阳极泥,以及有色冶炼与化工厂的酸泥。 [0003] The main raw material for the extraction of selenium smelters output anode mud, which in the first place is copper electrolysis anode slime, followed by nickel and lead electrolysis anode slime and mud acid and ferrous smelting chemical plant. 阳极泥和酸泥中富含较高含量的硒和碲,通过初步提前和冶炼,制成含硒为75 %以上的粗硒(一般称含硒大于75 %、小于98 %的硒产品为粗硒,粗硒中还含有5 %以下的碲),经过进一步的精炼提纯成为纯硒、高纯硒。 Anode slime and mud acid rich high content of selenium and tellurium, and advance through preliminary smelting, selenium is made 75% or more of crude selenium (generally referred selenium than 75%, less than 98% of the selenium as a crude product selenium, selenium crude also contains 5% tellurium), after further purification become refined pure selenium, selenium high purity. 国内每年纯硒、高纯硒的消耗量为1000~2000t,总量硒的80%以粗硒的方式在国内市场交易,作为纯硒、高纯硒加工厂的原料,交易量比较大。 Domestic annual net selenium, high purity selenium consumption of 1000 ~ 2000t, 80% of the total amount of selenium in a crude way of selenium in the domestic market trading, as pure selenium, selenium high purity raw materials processing plant, a greater amount of the transaction.

[0004] 目前,硒含量分析一般采用有色行业标准《YS/T 226. 12-2009硒化学分析方法第12部分:硒量的测定硫代硫酸钠容量法》,其原理是:试料用混合酸分解后,在硫酸介质中,用硫代硫酸钠标准溶液进行滴定。 [0004] Currently, the general analysis of selenium content in ferrous industry standard "YS / T 226. 12-2009 selenium chemical analysis methods - Part 12: Determination of the amount of sodium thiosulfate Se volumetric method", the principle is: mixing the sample with after the acid decomposition, in sulfuric acid was titrated with standard sodium thiosulfate solution. 临近终点时加入碘化钾,反应析出的碘以淀粉为指示剂,继续用硫代硫酸钠标准滴定液进行滴定,蓝色消失为终点。 Of potassium iodide was added towards the end, the reaction is precipitated iodine starch indicator and continue titration with standard sodium thiosulfate titration solution, blue color disappears as the end point. 其适用的测定范围: 98. 0%-99. 0%。 Measurement range which applies: 98.0% -990%. 粗硒没有相应、统一的分析方法,大都借鉴有色行业标准《YS/T 226. 12-2009 硒化学分析方法第12部分:硒量的测定硫代硫酸钠容量法》,但是粗硒不在其适用范围, 并且粗硒中的碲严重影响测定结果,导致争议和纠纷。 The crude no corresponding selenium, uniform analytical method, most non-ferrous industry standard reference "YS / T 226. 12-2009 selenium chemical analysis methods - Part 12: Determination of the amount of sodium thiosulfate Se volumetric method", but is not adapted crude selenium range, selenium tellurium and the crude seriously affect the measurement result, resulting in disputes and disputes.

发明内容 SUMMARY

[0005] 本发明要解决的技术问题是现有的对粗硒中硒含量的分析没有标准的分析方法, 且粗硒中的碲严重影响测定结果,为此提供一种分析粗硒中硒含量的方法。 [0005] The present invention is to solve the technical problems of existing methods of analysis no standard analysis of the crude selenium content of selenium, selenium tellurium and the crude seriously affect the measurement result, for this purpose the crude selenium provides an analytical Selenium Methods.

[0006] 本发明的技术方案是:一种分析粗硒中硒含量的方法,它包括以下步骤: [0006] aspect of the present invention is: A method for analysis of the crude selenium selenium content, comprising the steps of:

[0007] (1)、干燥试样,取粒度不大于0. 098mm的试样在100°C~105°C烘箱中干燥2h,并置于干燥器中冷却至室温; [0007] (1), drying the sample, taking the sample size not greater than 0. 098mm at 100 ° C ~ 105 ° C oven for 2h, and cooled to room temperature in a desiccator;

[0008] (2)、称样,称取2. Og步骤(1)中的试样记为mQ,精确至0· OOOlg ; [0008] (2), said sample, a sample was weighed in step 2. Og note (1) in the range mQ and, accurate to 0 · OOOlg;

[0009] (3)、测定,将步骤(2)中的试样置于500mL锥形烧瓶中,加入7mL硝酸,在70°C~ 80°C水浴上消解完全,再加21mL的盐酸,待溶解完全后,拿下自然冷却,将冷却后的溶液移入200mL容量瓶中,以水定容到200.0 OmL,摇匀; [0009] (3), measuring the sample in step (2) was placed in a 500mL Erlenmeyer flask, nitric acid is added 7mL, complete digestion at a 70 ° C ~ 80 ° C water bath, plus 21mL of hydrochloric acid to be after complete dissolution, scored cooled, the cooled solution is transferred to 200mL volumetric flask, constant volume of water to 200.0 OmL, shake;

[0010] (4)、将步骤(3)中的溶液干过滤到洗净干燥的三角烧杯中,弃去最初20mL滤液, 移取100.0 OmL滤液到500mL的三角烧杯中,再加60mL的盐酸,摇匀,慢慢滴加50mL的水合联氨,在低温上慢慢加热到溶液澄清,放置待其自然冷却; [0010] (4), dry the solution of step (3) washing the filter into the drying triangular beaker, 20mL initial filtrate was discarded, the filtrate is pipetted into an Erlenmeyer 100.0 OmL in 500mL beaker, together with 60mL of hydrochloric acid, shake slowly added dropwise 50mL of hydrazine hydrate, slowly heated to a low temperature in the solution is clear, cool place until their natural;

[0011] (5)、在100°C~105°C烘箱中干燥玻璃砂芯坩埚并恒重,再放置于干燥器中冷却到室温后,取出玻璃砂芯坩埚在电子天平上称重记为Hi1,精确至0.0 OOlg ; [0011] (5), at 100 ° C ~ 105 ° C oven dried crucible and glass frit constant weight, and put in a desiccator to cool to room temperature, remove the sand core glass crucible weighed on an electronic balance referred to as hi1, accurate to 0.0 OOlg;

[0012] (6)、安装好抽滤装置,用玻璃砂芯坩埚抽滤步骤(4)中最后得到的溶液,先用蒸馏水洗涤玻璃砂芯坩埚内抽滤得到的沉淀3~5次,以pH试纸测定滤液呈中性,再用5mL无水乙醇清洗,无水乙醇挥发后,把玻璃砂芯坩埚放在100°C~105°C烘箱中烘干并恒重,并置于干燥器中冷却至室温,在电子天平上称重,精确至0. 〇〇〇lg,得沉淀和砂芯坩埚合重记为m2; [0012] (6), suction means installed, was treated with a medium glass frit crucible suction step (4), the resulting precipitate to obtain a 3 to 5 times with the crucible inner glass frit suction filtration and washed with distilled water to Determination of the filtrate is neutral to pH paper, and then 5mL of anhydrous ethanol, the ethanol evaporated, the crucible is placed on a glass frit 100 ° C ~ 105 ° C and a constant weight in a drying oven, and placed in a desiccator cooled to room temperature, weighed on an electronic balance, accurate to 0.5 〇〇〇lg give precipitates and the combined weight of the sand core crucible referred to as M2;

[0013] (7)、收集步骤(6)中的抽滤后的滤液放入250mL容量瓶中,加入5mL硝酸,以水定容到250mL,摇匀,用ICP - AES光谱法测定滤液中Se的含量记为cSe; [0013] (7), collecting filtrate after step (6) into suction 250mL volumetric flask, was added 5mL of nitric acid, made up to 250mL with water, shake, by ICP - Determination filtrate Se AES Spectrometry the content of the note is cSe;

[0014] (8)、将步骤(6)中的装有沉淀的玻璃砂芯坩埚放入IOOmL平底烧杯中,加入50mL 盐酸,再加入IOmL硝酸,放在70°C~80°C水浴上加热使沉淀溶解完全,取下冷却后,移入200mL容量瓶中,以水洗涤玻璃砂芯坩锅和平底烧杯3~5次,以水定容到200mL,摇匀,用ICP - AES光谱法测定滤液中Te的含量记为cTe; [0014] (8), the step (6) is precipitated with a sintered glass crucible is placed IOOmL flat-bottom beaker, was added 50mL of hydrochloric acid, nitric acid was added IOmL, on 70 ° C ~ 80 ° C water bath to dissolve the precipitate completely, removed by ICP after cooling, transferred to 200mL volumetric flask with water sand core glass crucible flat bottom beaker was washed 3-5 times with water to 200mL volume, shake, - Determination filtrate AES Spectrometry the content of Te referred to as CTE;

[0015] (9)、计算硒的质量分数(%), [0015] (9), calculates the mass fraction of selenium (%),

[0016] [0016]

Figure CN103592197BD00041

[0017] 其中!!!。 [0017] wherein !!!. ,和m2单位为克,c Se和c Te单位为微克/毫升。 , And m2 in grams, c Se and c Te micrograms / ml.

[0018] 本发明的有益效果是试样经酸溶解,过滤,分离酸不溶元素干扰;水合联氨还原, 过滤,分离部分干扰元素;沉淀再经酸溶解,光谱仪测定碲,排除主要干扰元素;滤液经光谱仪测定硒含量,对分析结果进行补正。 [0018] Advantageous effects of the present invention is a sample was dissolved, filtered, and separating the acid-insoluble interfering effect by an acid; hydrazine hydrate reduction, filtering, separating partial interference element; pellet was subjected to acid dissolution, spectrometer tellurium, exclusion of major interfering elements; The filtrate was measured by the spectrometer selenium content of the analysis result is corrected. 方法采用经典的重量法测定,消除主要干扰元素, ICP - AES光谱法补正滤液硒的损失,方法结果准确可靠,分析范围广,不但可以测定粗硒, 还可以测定硒含量在99. 9 %以下的纯硒,具有较大的推广价值。 Methods Determination of weight classical, mainly to eliminate interfering elements, ICP - accurate and filtrate loss corrected selenium AES spectroscopy, the results of the method, a wide range of analysis, not only coarse measurement of selenium, selenium content can also be determined at 99.9% or less pure selenium, with great promotional value.

具体实施方式 detailed description

[0019] 下面结合具体实施方式对本发明做进一步说明。 [0019] DETAILED DESCRIPTION The following embodiments of the present invention will be further described.

[0020] 实施例1 :(1)、干燥试样,取粒度0. 098mm的试样在100°C烘箱中干燥2h,并置于干燥器中冷却至室温; [0020] Example 1: (1), drying the sample, the sample size taken 0. 098mm in 100 ° C oven for 2h, and cooled to room temperature in a desiccator;

[0021] (2)、称样,称取2. Og步骤(1)中的试样记为m。 [0021] (2), said sample, a sample was weighed in step 2. Og note (1) is m. ,精确至0· OOOlg ; , Accurate to 0 · OOOlg;

[0022] (3)、测定,将步骤(2)中的试样置于500mL锥形烧瓶中,加入7mL硝酸,在70°C 水浴上消解完全,再加21mL的盐酸,待溶解完全后,拿下自然冷却,将冷却后的溶液移入200mL容量瓶中,以水定容到200. 00mL,摇匀; [0022] (3), the measurement, the sample (2) was placed in a 500mL conical flask step, nitric acid was added 7mL, complete digestion at 70 ° C on a water bath, plus 21mL of hydrochloric acid to be dissolved completed, scored cooled, the cooled solution is transferred to 200mL volumetric flask, constant volume of water to 200. 00mL, shake;

[0023] (4)、将步骤(3)中的溶液干过滤到洗净干燥的三角烧杯中,弃去最初20mL滤液, 移取100.0 OmL滤液到500mL的三角烧杯中,再加60mL的盐酸,摇匀,慢慢滴加50mL的水合联氨,在低温上慢慢加热到溶液澄清,放置待其自然冷却; [0023] (4), dry the solution of step (3) washing the filter into the drying triangular beaker, 20mL initial filtrate was discarded, the filtrate is pipetted into an Erlenmeyer 100.0 OmL in 500mL beaker, together with 60mL of hydrochloric acid, shake slowly added dropwise 50mL of hydrazine hydrate, slowly heated to a low temperature in the solution is clear, cool place until their natural;

[0024] (5)、在KKTC烘箱中干燥玻璃砂芯坩埚并恒重,再放置于干燥器中冷却到室温后, 取出玻璃砂芯坩埚在电子天平上称重记为Hi1,精确至0.0 OOlg ; [0024] (5), dried in an oven KKTC sintered glass crucible and a constant weight in a desiccator then be enclosed cooled to room temperature, remove the sand core glass crucible weighed on an electronic balance referred to as Hi1 of, accurate to 0.0 OOlg ;

[0025] (6)、安装好抽滤装置,用玻璃砂芯坩埚抽滤步骤(4)中最后得到的溶液,先用蒸馏水洗涤玻璃砂芯坩埚内抽滤得到的沉淀3次,以pH试纸测定滤液呈中性,再用5mL无水乙醇清洗,无水乙醇挥发后,把玻璃砂芯坩埚放在100 °C烘箱中烘干并恒重,并置于干燥器中冷却至室温,在电子天平上称重,精确至0. 〇〇〇lg,得沉淀和砂芯坩埚合重记为m2; [0025] (6), suction means installed with a sintered glass crucible by suction filtration step (4) in the resulting solution, first with the crucible inner glass frit suction filtration and washed with distilled water to give precipitated 3 times to pH paper Determination of the filtrate became neutral, and then 5mL of anhydrous ethanol, the ethanol evaporated, the glass frit 100 ° C, was placed in an oven and dried to constant weight, placed in a desiccator and cooled to room temperature, the electronic weighed on a balance, accurate to 0.5 〇〇〇lg give precipitates and the combined weight of the sand core crucible referred to as M2;

[0026] (7)、收集步骤(6)中的抽滤后的滤液放入250mL容量瓶中,加入5mL硝酸,以水定容到250mL,摇匀,用ICP - AES光谱法测定滤液中Se的含量记为cSe; [0026] (7), collecting filtrate after step (6) into suction 250mL volumetric flask, was added 5mL of nitric acid, made up to 250mL with water, shake, by ICP - Determination filtrate Se AES Spectrometry the content of the note is cSe;

[0027] (8)、将步骤(6)中的装有沉淀的玻璃砂芯坩埚放入IOOmL平底烧杯中,加入50mL 盐酸,再加入IOmL硝酸,放在70°C水浴上加热使沉淀溶解完全,取下冷却后,移入200mL容量瓶中,以水洗涤玻璃砂芯坩锅和平底烧杯3次,以水定容到200mL,摇匀,用ICP - AES光谱法测定滤液中Te的含量记为cTe; [0027] (8), the step (6) is precipitated with a sintered glass crucible is placed IOOmL flat-bottom beaker, was added 50mL of hydrochloric acid, nitric acid was added IOmL, on a 70 ° C water bath to dissolve the precipitate completely after removing the cooling, transferred to 200mL volumetric flask, washed with water glass frit crucible flat bottom beaker three times, made up to 200mL with water, shake, by ICP - AES Spectrometry Te content referred to as filtrate cTe;

[0028] (9)、计算硒的质量分数(%), [0028] (9), calculates the mass fraction of selenium (%),

[0029] [0029]

Figure CN103592197BD00051

[0030] 其中mQ、mJP m2单位为克,c Se和c Te单位为微克/毫升。 [0030] wherein mQ, mJP m2 in grams, c Se and c Te micrograms / ml.

[0031] 实施例2 :(1)、干燥试样,取粒度为0.090mm的试样在105°C烘箱中干燥2h,并置于干燥器中冷却至室温; [0031] Example 2: (1) drying a sample, a sample size taken 0.090mm in 105 ° C oven for 2h, and cooled to room temperature in a desiccator;

[0032] (2)、称样,称取2. Og步骤(1)中的试样记为mQ,精确至0· OOOlg ; [0032] (2), said sample, a sample was weighed in step 2. Og note (1) in the range mQ and, accurate to 0 · OOOlg;

[0033] (3)、测定,将步骤(2)中的试样置于500mL锥形烧瓶中,加入7mL硝酸,在80°C 水浴上消解完全,再加21mL的盐酸,待溶解完全后,拿下自然冷却,将冷却后的溶液移入200mL容量瓶中,以水定容到200.0 OmL,摇匀; [0033] (3), the measurement, the sample (2) was placed in a 500mL conical flask step, nitric acid was added 7mL, complete digestion at 80 ° C on a water bath, plus 21mL of hydrochloric acid to be dissolved completed, scored cooled, the cooled solution is transferred to 200mL volumetric flask, constant volume of water to 200.0 OmL, shake;

[0034] (4)、将步骤(3)中的溶液干过滤到洗净干燥的三角烧杯中,弃去最初20mL滤液, 移取100.0 OmL滤液到500mL的三角烧杯中,再加60mL的盐酸,摇匀,慢慢滴加50mL的水合联氨,在低温上慢慢加热到溶液澄清,放置待其自然冷却; [0034] (4), dry the solution of step (3) washing the filter into the drying triangular beaker, 20mL initial filtrate was discarded, the filtrate is pipetted into an Erlenmeyer 100.0 OmL in 500mL beaker, together with 60mL of hydrochloric acid, shake slowly added dropwise 50mL of hydrazine hydrate, slowly heated to a low temperature in the solution is clear, cool place until their natural;

[0035] (5)、在105°C烘箱中干燥玻璃砂芯坩埚并恒重,再放置于干燥器中冷却到室温后, 取出玻璃砂芯坩埚在电子天平上称重记为Hi1,精确至0.0 OOlg ; [0035] (5), at 105 ° C in an oven dried crucible and glass frit constant weight, then be enclosed in a desiccator cooled to room temperature, remove the sand core glass crucible Weighing Hi1 denoted on the electronic balance accurate to 0.0 OOlg;

[0036] (6)、安装好抽滤装置,用玻璃砂芯坩埚抽滤步骤(4)中最后得到的溶液,先用蒸馏水洗涤玻璃砂芯坩埚内抽滤得到的沉淀5次,以pH试纸测定滤液呈中性,再用5mL无水乙醇清洗,无水乙醇挥发后,把玻璃砂芯坩埚放在l〇5°C烘箱中烘干并恒重,并置于干燥器中冷却至室温,在电子天平上称重,精确至0. 〇〇〇lg,得沉淀和砂芯坩埚合重记为m2; [0036] (6), suction means installed with a sintered glass crucible by suction filtration step (4) in the resulting solution, first with the crucible inner glass frit suction filtration and washed with distilled water five times resulting precipitate to pH paper Determination of the filtrate became neutral, and then 5mL of anhydrous ethanol, the ethanol evaporated, the glass frit l〇5 ° C, was placed in an oven and dried to constant weight, placed in a desiccator and cooled to room temperature, on an electronic weighing scales, accurate to 0. 〇〇〇lg give precipitates and the combined weight of the sand core crucible referred to as M2;

[0037] (7)、收集步骤(6)中的抽滤后的滤液放入250mL容量瓶中,加入5mL硝酸,以水定容到250mL,摇匀,用ICP - AES光谱法测定滤液中Se的含量记为cSe; [0037] (7), collecting filtrate after step (6) into suction 250mL volumetric flask, was added 5mL of nitric acid, made up to 250mL with water, shake, by ICP - Determination filtrate Se AES Spectrometry the content of the note is cSe;

[0038] (8)、将步骤(6)中的装有沉淀的玻璃砂芯坩埚放入IOOmL平底烧杯中,加入50mL 盐酸,再加入IOmL硝酸,放在80°C水浴上加热使沉淀溶解完全,取下冷却后,移入200mL容量瓶中,以水洗涤玻璃砂芯坩锅和平底烧杯5次,以水定容到200mL,摇匀,用ICP - AES光谱法测定滤液中Te的含量记为cTe; [0038] (8), the step (6) is precipitated with a sintered glass crucible is placed IOOmL flat-bottom beaker, was added 50mL of hydrochloric acid, nitric acid was added IOmL, on a 80 ° C water bath to dissolve the precipitate completely after removing the cooling, transferred to 200mL volumetric flask, washed with water glass frit crucible flat bottom beaker five times, made up to 200mL with water, shake, by ICP - AES Spectrometry Te content referred to as filtrate cTe;

[0039] (9)、计算硒的质量分数(%), [0039] (9), calculates the mass fraction of selenium (%),

[0040] [0040]

Figure CN103592197BD00061

[0041] 其中mQ、mjP m2单位为克,c Se和c Te单位为微克/毫升。 [0041] wherein mQ, mjP m2 in grams, c Se and c Te micrograms / ml.

[0042] 上面结合实施例对本发明进行了示例性描述,显然本发明具体实现并不受上述方式的限制,只要采用了本发明的方法构思和技术方案进行的各种非实质性的改进,或未经改进将本发明的构思和技术方案直接应用于其它场合的,均在本发明的保护范围之内。 [0042] The above examples of the embodiments in conjunction with the present invention has been exemplarily described, the present invention is embodied clearly not limited to the above embodiment, as long as using a variety of methods insubstantial modifications spirit and aspect of the present invention is carried out, or the unmodified and the technical concept of the present invention is directly applicable to other applications, it is within the scope of the present invention.

Claims (1)

  1. 1. 一种分析粗硒中硒含量的方法,其特征是它包括以下步骤: (1) 、干燥试样,取粒度不大于0. 098mm的试样在100°C~105°C烘箱中干燥2h,并置于干燥器中冷却至室温; (2) 、称样,称取2. 0g步骤(1)中的试样记为mQ,精确至0•OOOlg; (3) 、测定,将步骤(2)中的试样置于500mL锥形烧瓶中,加入7mL硝酸,在70°C~80°C 水浴上消解完全,再加21mL的盐酸,待溶解完全后,拿下自然冷却,将冷却后的溶液移入200mL容量瓶中,以水定容到200.OOmL,摇匀; (4) 、将步骤(3)中的溶液干过滤到洗净干燥的三角烧杯中,弃去最初20mL滤液,移取100. 00mL滤液到500mL的三角烧杯中,再加60mL的盐酸,摇匀,慢慢滴加50mL的水合联氨, 在低温上慢慢加热到溶液澄清,放置待其自然冷却; (5) 、在100°C~105°C烘箱中干燥玻璃砂芯坩埚并恒重,再放置于干燥器中冷却到室温后,取出玻璃砂芯坩埚在 1. A method of crude selenium selenium content analysis, characterized in that it comprises the following steps: (1), drying the sample, taking the sample size not greater than 0. 098mm was dried at 100 ° C ~ 105 ° C oven 2h, cooled and placed in a desiccator to room temperature; (2), said sample, a sample was weighed in step 2. 0g note (1) in the range mQ and, accurate to 0 • OOOlg; (3), measured in step sample (2) was placed in a 500mL Erlenmeyer flask, nitric acid is added 7mL, complete digestion at a 70 ° C ~ 80 ° C water bath, plus 21mL of hydrochloric acid to be dissolved completely, scored natural cooling, cooling after the solution is transferred to 200mL volumetric flask, constant volume of water to 200.OOmL, shake; (4), dry the solution of step (3) washing the filter into the drying triangular beaker, 20mL initial filtrate was discarded, the filtrate was pipetted into an Erlenmeyer 100. 00mL beaker of 500mL, plus 60mL of hydrochloric acid, shake slowly added dropwise 50mL of hydrazine hydrate, slowly heated to a clear solution at low temperature, natural cooling until their place; (5 ) at 100 ° C ~ 105 ° C oven dried crucible and glass frit constant weight, then be enclosed in a desiccator cooled to room temperature, remove the sand core glass crucible 电子天平上称重记为叫,精确至0.OOOlg; (6) 、安装好抽滤装置,用玻璃砂芯坩埚抽滤步骤(4)中最后得到的溶液,先用蒸馏水洗涤玻璃砂芯坩埚内抽滤得到的沉淀3~5次,以pH试纸测定滤液呈中性,再用5mL无水乙醇清洗,无水乙醇挥发后,把玻璃砂芯坩埚放在l〇〇°C~105°C烘箱中烘干并恒重,并置于干燥器中冷却至室温,在电子天平上称重,精确至0. 〇〇〇lg,得沉淀和砂芯坩埚合重记为m2; (7) 、收集步骤(6)中的抽滤后的滤液放入250mL容量瓶中,加入5mL硝酸,以水定容到250mL,摇匀,用ICP-AES光谱法测定滤液中Se的含量记为cSe; (8 )、将步骤(6 )中的装有沉淀的玻璃砂芯坩埚放入100mL平底烧杯中,加入50mL盐酸, 再加入10mL硝酸,放在70°C~80°C水浴上加热使沉淀溶解完全,取下冷却后,移入200mL 容量瓶中,以水洗涤玻璃砂芯坩锅和平底烧杯3~5次,以水定容到200mL Referred to as weighed on an electronic balance is called the nearest 0.OOOlg; (6), suction means installed with a sintered glass crucible by suction filtration step (4) in the final solution was obtained, the first glass frit and washed with distilled water crucible after filtration the precipitate obtained 3 to 5 times, the pH test paper and the filtrate is neutral, and then 5mL of anhydrous ethanol, the ethanol evaporated, the sand core glass crucible placed l〇〇 ° C ~ 105 ° C and a constant weight in a drying oven, and cooled to room temperature in a desiccator, weighed on an electronic balance accurate to 0. 〇〇〇lg give precipitates and the combined weight of the sand core crucible referred to as M2; (. 7), the filtrate was collected after step (6) into suction 250mL volumetric flask, was added 5mL of nitric acid, made up to 250mL with water, shake well, the content of Se in the filtrate was referred to ICP-AES spectroscopy of CSE; ( 8), step 6) (sintered glass containing precipitated 100mL crucible into flat-bottom beaker, was added 50mL of hydrochloric acid, 10mL of nitric acid was added, placed on 70 ° C ~ 80 ° C water bath to dissolve the precipitate completely after removing the cooling, transferred to 200mL volumetric flask with water sand core glass crucible flat bottom beaker was washed 3-5 times with water to 200mL volume 摇匀,用ICP- AES光谱法测定滤液中Te的含量记为cTe; (9)、计算硒的质量分数, Shake the filtrate referred to as cTe Te content was determined by ICP- AES spectroscopy; (9), calculates the mass fraction of selenium,
    Figure CN103592197BC00021
    其中nvmdPm2单位为克,cSe和cTe单位为微克/毫升。 Wherein nvmdPm2 in grams, cSe and cTe micrograms / ml.
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