CN111638101A - 一种同时测定锂矿石中锂钙含量的湿法碱熔方法 - Google Patents
一种同时测定锂矿石中锂钙含量的湿法碱熔方法 Download PDFInfo
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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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- 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
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Abstract
一种同时测定锂矿石中锂钙含量的湿法碱熔方法,利用电感耦合等离子体发射光谱仪测定,电感耦合等离子体发射光谱仪测定用试样溶液的制备方法是:(1)称取干燥过的样品,置于坩埚中,在样品上平铺氢氧化钠;(2)给坩埚加盖,加热至样品熔融,保温,取出,冷却至熔融物凝固;(3)将坩埚和盖放入装有热水的反应器中浸提,用稀盐酸洗净坩埚和盖;(4)加浓盐酸,冷却至室温;(5)稀释;(6)干过滤,稀释,即成。本发明采用NaOH碱熔制备样品,避免使用氢氟酸和易爆品高氯酸;利用锂、钙元素易电离易激发的特点,采用电感耦合等离子体发射光谱仪(ICP‑AES)直接测定锂矿石中锂钙含量:本发明操作简单,检测范围宽。
Description
技术领域
本发明涉及一种测定锂钙含量的湿法碱熔方法,具体涉及一种测定锂矿石中锂钙含量的湿法碱熔方法。
背景技术
锂辉石是主要的含锂矿石之一,是制取碳酸锂和氢氧化锂的主要固相原料。由于大部分的锂辉石品位较低,利用前需要进行选矿富集。
目前,锂辉石的主要选矿方法为正浮选法,即以碳酸钠和氢氧化钠为pH调整剂,钙离子、铅离子等离子为活化剂,脂肪酸皂及其衍生物为捕收剂,浮选矿石中的锂辉石矿物。然而,当矿石中含有含钙矿物时,由于含钙矿物在碱性条件下可浮性优于锂辉石,含钙矿石优先富集到精矿中,导致浮选指标不理想,因此锂辉石中钙元素的含量是评价矿石质量、提锂工艺的重要指标,能同时快速准确地提供矿石中锂钙含量在锂矿石提锂研究中极为重要。
目前,锂矿石中锂的标准分析方法是GB/T 17413.1-2010 锂矿石、铷矿石、铯矿石化学分析方法第1部分:锂量测定原子吸收法,该法试样分解采用三酸消解,需要使用氢氟酸和易爆品高氯酸,存在试剂用量大、试剂危险系数高等缺点。
张豫红发表在“中国电子学会生产技术学会理化分析四届年会”(1991年,太原)中的“锂辉石中常量锂微量钠钾钙镁的原子吸收光谱测定”公开了锂矿石中钙含量的分析方法,该法一次只能分析一种元素,不能同时测定锂元素。
韩晓发表在《中国无机分析化学》(2019年4月,第9卷第2期)中“EDTA络合滴定法快速测定矿石中钙、镁”,该络合滴定法适用于常量分析,不适合微量分析。
庞海榕等人发表在《核电子学与探测技术》(2017年2月,第37卷第2期)中的“EDXRF法测定石灰岩矿中Ca含量”公开了能量色散X射线荧光光谱(EDXRF)法测定石灰岩矿中Ca含量的分析方法,该法对含量低的元素因其特征X射线荧光能量不高,产额少,不易被EDXRF光谱仪激发或直接探测得到,使这一技术在低品位矿石中钙含量的测定应用受到限制。
发明内容
本发明所要解决的技术问题是,克服现有技术存在的上述缺陷,提供一种不使用氢氟酸和高氯酸,精确度高,适用于微量分析的同时测定锂矿石中锂钙含量的湿法碱熔方法。
本发明解决其技术问题所采用的技术方案如下:一种同时测定锂矿石中锂钙含量的湿法碱熔方法,利用电感耦合等离子体发射光谱仪测定,电感耦合等离子体发射光谱仪测定用试样溶液的制备,包括以下步骤:
(1)称取干燥过的样品,置于坩埚中,在样品上平铺氢氧化钠;
(2)给坩埚加盖,加热至样品熔融,保温,取出,冷却至熔融物凝固;
(3)将坩埚和盖放入装有热水的反应器中浸提,用稀盐酸洗净坩埚和盖,洗液留在反应器中,移出坩埚和盖;
(4)加浓盐酸,使反应器中液体澄清,冷却至室温;
(5)将反应器的液体加水稀释,摇匀,静置;
(6)干过滤,移取滤液,加浓盐酸,加水稀释,即成。
优选地,步骤(1)中,所述样品的粒度为200目以上。
优选地,步骤(1)中,称取样品的精度为万分之一克。
优选地,步骤(1)中,所述坩埚为银坩埚。
优选地,步骤(1)中,所述氢氧化钠与样品的质量比为7~12:1,氢氧化钠与样品的反应方程式可简写为:
由反应方程式再结合反应物的密度,可以计算出锂矿石与氢氧化钠反应的质量比为1比1.2,为使矿石反应充分,氢氧化钠需过量7到10倍。
优选地,步骤(2)中,所述加热为加热至600~650 ℃,该温度下,坩埚内的固体能够熔融,充分反应。
优选地,步骤(2)中,所述保温的时间为20~30 min。
优选地,步骤(3)中,所述稀盐酸的质量百分比为3~10%,以充分中和坩埚上的碱。
优选地,步骤(4)中,所述浓盐酸与氢氧化钠的用量比为7~5 mL:1g,用于保证溶液的pH值在1以下,锂、钙等以离子形式存在。
优选地,步骤(4)中,加浓盐酸时加热促进液体澄清。
优选地,步骤(5)中,所述加水稀释,按照每1g样品配制成1200~1400 mL溶液的比例进行。
优选地,步骤(6)中,所述浓盐酸的用量为稀释完毕后最终体积的3%~5%,以保证溶液是一个酸性体系,溶液中的锂离子、钙离子均能稳定存在。
优选地,步骤(6)中,所述加水稀释的稀释倍数为20~28倍。该稀释倍数可以最大限度地减少引入的酸和碱带来的基底干扰。
本发明有益效果:(1)采用NaOH碱熔制备样品,不但避免了常规方法三酸消解中要使用氢氟酸和易爆品高氯酸的缺陷,而且比常规分解试样方法所耗时间缩短了二分之一;(2)利用锂、钙元素易电离易激发的特点,采用电感耦合等离子体发射光谱仪(ICP-AES)直接测定锂矿石中锂钙含量,利用二级稀释消除光谱干扰和背景干扰,能同时测定两种元素:(3)本发明操作简单,检测范围宽,锂的测定范围为0.06%至20%,钙的测定范围为0.05%至20%。
具体实施方式
以下结合实施例对本发明作进一步说明。
本发明各实施例同时测定锂矿石中锂钙含量使用的湿法碱熔方法如下。
1仪器
FA2004电子分析天平(上海恒平科学仪器有限公司);
iCAP6000系列电感耦合等离子体发射光谱仪(美国赛默飞公司),配有高盐进样包,氩气加湿器;
ASX-260 Autosampler全自动进样器(美国赛默飞公司);
2试剂:
锂矿石GBW07152(国家标准物质研究中心);锂矿石GBW07153(国家标准物质研究中心);GSB G 62003-91(0501)锂元素标准溶液(国家钢铁材料测试中心钢铁研究院);GSB04-1720-2004钙元素标准溶液(国家有色金属电子材料分析测试中心);盐酸(AR);氢氧化钠(AR)。除非另有说明,本实验用水为电阻率达到18.25MΩ的超纯水。
根据样品中Li、Ca的含量,配制一系列百分比浓度由低到高的标准溶液,溶液中元素含量见表1。
表1标准系列溶液
标准溶液编号 | 空白 | 1 | 2 | 3 | 4 | 5 |
Ca浓度(mg/L) | 0.00 | 0.02 | 0.20 | 1.00 | 5.00 | 10.0 |
Li浓度(mg/L) | 0.00 | 0.01 | 0.10 | 1.00 | 5.00 | 10.0 |
3离子源和分析参数设置
本方法主要研究的锂、钙元素属于碱金属和碱土金属,其有易激发和易电离的特点,根据其特点设置等离子源,虽然所有谱线强度都随功率的增加而增加,但功率过大会带来背景辐射增强,信背比变差,综合比较选择功率为1150W,其它设置根据功率做相应的调整,具体见表2和表3。
表2 等离子源设置
功率(W) | 雾化器气体流量(L/min) | 辅助气(L/min) | 垂直观测高度(mm) | 分析泵速(rmp) | 分析泵速(rmp) | 泵稳定时间(S) |
1150 | 0.6 | 0.5 | 12 | 50 | 100 | 5 |
表3 分析参数设置
4 谱线与谱图设置
本方法应用谱线和谱图宽度以及背景扣除位置见表4。
表4 谱线和谱图设置
元素 | 波长(nm) | 谱图宽度 | 背景扣除位置 |
Li | 670.784 | 2格 | 左背景(393.366nm),右背景(393.399nm) |
Ca | 393.366 | 2格 | 左背景(670.712nm),右背景(670.856nm) |
5 试样处理
准确称取0.2g(精确至0.0001g)干燥过200目筛的试样,置于银坩埚中,在样品上平铺2g氢氧化钠,加盖放入马弗炉中,从低温升至620℃,并保温熔融25min,取出冷却(待熔融物冷却至凝固状态),将银坩埚和盖放入装有50ml热水的250ml烧杯中浸提,用质量百分比5%盐酸洗出坩埚和盖,补加浓盐酸12ml,加热,使盐类溶解至澄清。冷却至室温,转入250.00mL塑料容量瓶中,用水定容至刻度,摇匀,静置。干过滤,移取2.00毫升滤液于50.00ml塑料容量瓶中(进行二级稀释),补加1ml浓盐酸,用水定容至刻度,摇匀,得到用ICP-AES测定用试样溶液。
实施例1
称取国家标准物质GBW07152和GBW07153各3份,按试样前处理方法处理得到测定用试样溶液,按前述仪器设置条件分析矿石中锂钙含量,得到方法准确度,结果见表5。
表5 方法准确度
由表可知,锂含量相对误差小于2%;钙含量相对误差小于10%。
实施例2
将本方法应用于三门峡某锂矿石提锂试验研究中500余个样品的测定,取其中部分样品按试样前处理方法处理得到测定用试样溶液,按前述仪器设置条件分析矿石中锂钙含量,做精密度测试试验,数据见表6。
表6 方法精密度
由表中数据可知,锂相对标准偏差(RSD)小于2;钙相对标准偏差(RSD)小于2,说明本方法精密度高。
Claims (7)
1.一种同时测定锂矿石中锂钙含量的湿法碱熔方法,其特征在于,利用电感耦合等离子体发射光谱仪测定,电感耦合等离子体发射光谱仪测定用试样溶液的制备,包括以下步骤:
(1)称取干燥过的样品,置于坩埚中,在样品上平铺氢氧化钠;
(2)给坩埚加盖,加热至样品熔融,保温,取出,冷却至熔融物凝固;
(3)将坩埚和盖放入装有热水的反应器中浸提,用稀盐酸洗净坩埚和盖,洗液留在反应器中,移出坩埚和盖;
(4)加浓盐酸,使反应器中液体澄清,冷却至室温;
(5)将反应器的液体加水稀释,摇匀,静置;
(6)干过滤,移取滤液,加浓盐酸,加水稀释,即成。
2.根据权利要求1所述的同时测定锂矿石中锂钙含量的湿法碱熔方法,其特征在于,步骤(1)中,所述样品的粒度为200目以上;称取样品的精度为万分之一克;所述坩埚为银坩埚;所述氢氧化钠与样品的质量比为7~12:1。
3. 根据权利要求1或2所述的同时测定锂矿石中锂钙含量的湿法碱熔方法,其特征在于,步骤(2)中,所述加热为加热至600~650 ℃;所述保温的时间为20~30 min。
4.根据权利要求1~3之一所述的同时测定锂矿石中锂钙含量的湿法碱熔方法,其特征在于,步骤(3)中,所述稀盐酸的质量百分比为3~10%。
5. 根据权利要求1~4之一所述的同时测定锂矿石中锂钙含量的湿法碱熔方法,其特征在于,步骤(4)中,所述浓盐酸与氢氧化钠的用量比为7~5 mL:1 g;加浓盐酸时加热促进液体澄清。
6. 根据权利要求1~5之一所述的同时测定锂矿石中锂钙含量的湿法碱熔方法,其特征在于,步骤(5)中,所述加水稀释,按照每1g样品配制成1200~1400 mL溶液的比例进行。
7.根据权利要求1~6之一所述的同时测定锂矿石中锂钙含量的湿法碱熔方法,其特征在于,步骤(6)中,所述浓盐酸的用量为稀释完毕后最终体积的3%~5%;所述加水稀释的稀释倍数为20~28倍。
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113447473A (zh) * | 2021-06-28 | 2021-09-28 | 中蓝长化工程科技有限公司 | 一种用微波碱消解检测硅酸盐中元素含量的方法 |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101581638A (zh) * | 2009-06-01 | 2009-11-18 | 中国铝业股份有限公司 | 一水硬铝石型铝土矿生产氧化铝的固体试样的熔融方法 |
CN102053066A (zh) * | 2009-11-09 | 2011-05-11 | 北京有色金属研究总院 | 一种矿石样品中铬的分析方法 |
CN102213704A (zh) * | 2011-03-30 | 2011-10-12 | 太原重工股份有限公司 | 硅钙合金中硅钙元素含量的测定法 |
CN102636485A (zh) * | 2012-03-28 | 2012-08-15 | 云南磷化集团有限公司 | 一种测定铁矿石中氧化钙含量的方法 |
CN106338505A (zh) * | 2016-08-22 | 2017-01-18 | 中国铝业股份有限公司 | 一种测定赤泥中的稀土含量的方法 |
CN106979879A (zh) * | 2017-05-11 | 2017-07-25 | 方大特钢科技股份有限公司 | Icp光谱仪分析铁矿石中有害元素的熔融制样方法 |
CN108645995A (zh) * | 2018-04-28 | 2018-10-12 | 宜春市金地锂业有限公司 | 用于锂云母选矿后的矿石质量检测装置及检测方法 |
-
2020
- 2020-05-08 CN CN202010382397.0A patent/CN111638101A/zh active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101581638A (zh) * | 2009-06-01 | 2009-11-18 | 中国铝业股份有限公司 | 一水硬铝石型铝土矿生产氧化铝的固体试样的熔融方法 |
CN102053066A (zh) * | 2009-11-09 | 2011-05-11 | 北京有色金属研究总院 | 一种矿石样品中铬的分析方法 |
CN102213704A (zh) * | 2011-03-30 | 2011-10-12 | 太原重工股份有限公司 | 硅钙合金中硅钙元素含量的测定法 |
CN102636485A (zh) * | 2012-03-28 | 2012-08-15 | 云南磷化集团有限公司 | 一种测定铁矿石中氧化钙含量的方法 |
CN106338505A (zh) * | 2016-08-22 | 2017-01-18 | 中国铝业股份有限公司 | 一种测定赤泥中的稀土含量的方法 |
CN106979879A (zh) * | 2017-05-11 | 2017-07-25 | 方大特钢科技股份有限公司 | Icp光谱仪分析铁矿石中有害元素的熔融制样方法 |
CN108645995A (zh) * | 2018-04-28 | 2018-10-12 | 宜春市金地锂业有限公司 | 用于锂云母选矿后的矿石质量检测装置及检测方法 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113447473A (zh) * | 2021-06-28 | 2021-09-28 | 中蓝长化工程科技有限公司 | 一种用微波碱消解检测硅酸盐中元素含量的方法 |
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