CN116337980A - 一种铜精矿中金银的测定方法 - Google Patents
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 63
- 239000004332 silver Substances 0.000 title claims abstract description 63
- 239000010931 gold Substances 0.000 title claims abstract description 51
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000012141 concentrate Substances 0.000 title claims abstract description 25
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 25
- 239000010949 copper Substances 0.000 title claims abstract description 25
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 62
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012086 standard solution Substances 0.000 claims abstract description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960000583 acetic acid Drugs 0.000 claims abstract description 8
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052951 chalcopyrite Inorganic materials 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- 238000005259 measurement Methods 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 241000416536 Euproctis pseudoconspersa Species 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000013062 quality control Sample Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
本发明涉及金属检测技术领域,具体涉及一种铜精矿中金银的测定方法。具体技术方案为:一种铜精矿中金银的测定方法,包括以下步骤:(1)在铜精矿中加入钯标准溶液,得到银合粒;(2)将银合粒加入到冰乙酸中加热,捞出清洗,烘干;(3)将银合粒加入到浓硝酸中,加热溶解后,再加入浓盐酸直至沉淀完全溶解,加热蒸干;(4)加入王水,加热至溶液澄清,冷却后定容,测量金银。本发明解决了现有技术中样品中银含量低无法测量的问题。
Description
技术领域
本发明涉及金属检测技术领域,具体涉及一种铜精矿中金银的测定方法。
背景技术
在测定铜精矿金银的过程中,一般采用火试金分离富集后,重量法或仪器测定金,容量法测定银,但是,当样品中银含量很低时,火试金得到的合粒太小,在操作时无法夹取,或者当合粒中银与金的比例小于3时,合粒中银不能完全被溶解,影响分金。针对这种情况,传统的方法是原子吸收测定银,火试金补加银后测定金。由于无法预先判断样品中银的含量高低,往往需要返工。因此,通过一次试金实现金银联测,对实际工作有十分重要的意义。
发明内容
针对现有技术的不足,本发明提供了一种铜精矿中金银的测定方法,解决了现有技术中样品中银含量低无法测量的问题。
为实现以上目的,本发明通过以下技术方案予以实现:
本发明公开了一种铜精矿中金银的测定方法,包括以下步骤:
(1)在铜精矿中加入钯标准溶液,得到银合粒;
(2)将银合粒加入到冰乙酸中加热,捞出清洗,烘干;
(3)将银合粒加入到浓硝酸中,加热溶解后,再加入浓盐酸直至沉淀完全溶解,加热蒸干;
(4)加入王水,加热至溶液澄清,冷却后定容,测量金银。
优选的,所述钯标准溶液的浓度为0.8g/L~2g/L。
优选的,所述金铜矿与钯标准溶液的用量比为75000:1~37500:1。
优选的,冰乙酸的用量为15~25mL。
优选的,浓硝酸的用量为5~10mL。
优选的,王水的用量为2~5mL。
本发明具备以下有益效果:
本发明通过一次试金分离富集金银,选择火试金—ICP-AES测定金和杂质,减杂法测定银,实现金银联测,这对于提高铜精矿分析速度、减少分析环节。
具体实施方式
下面将结合本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
若未特别指明,实施举例中所用的技术手段为本领域技术人员所熟知的常规手段。
本发明公开了一种铜精矿中金银的测定方法,包括以下步骤:
(1)在铜精矿中加入钯标准溶液,得到银合粒;
(2)将银合粒加入到冰乙酸中加热,捞出清洗,烘干;
(3)将银合粒加入到浓硝酸中,加热溶解后,再加入浓盐酸直至沉淀完全溶解,加热蒸干;
(4)加入王水,加热至溶液澄清,冷却后定容,测量金银。
其中,所述钯标准溶液的浓度为0.8g/L~2g/L。所述金铜矿与钯标准溶液的用量比为75000:1~37500:1。冰乙酸的用量为15~25mL。浓硝酸的用量为5~10mL。
通过发明人研究发现:钯,在试金中能被富集在合粒中,且其化学性质与银有相似之处,即在硝酸中能被溶解,因此在配料中加入少量的钯,可以代替银增加合粒的质量,保证合粒能够方便夹取,同时钯易溶解于硝酸与金分离而不影响金的溶解。而且,钯量不需要准确加入,因为,合粒中增加的重量,可以通过对合粒中钯进行测定,然后从合粒质量中减去,降低操作难度。因此选择在配料中加入钯,能解决样品中银含量低问题。
基于以上情况,拟按照测定金时的称样量,通过一次试金分离富集金银,选择火试金—ICP-AES测定金和杂质,减杂法测定银,实现金银联测。
铜精矿中金银的测定方法包括以下步骤:
(1)称取15g铜精矿,在配料中加入钯标准溶液(1g/L)2~4滴,得到银合粒。
(2)将合粒砸扁后,置于30mL瓷坩埚中。加15mL冰乙酸,加热微沸至5mL,排出溶液,用热水将合粒清洗3次,烤干,冷却后称量合粒的质量。
(3)将合粒置于100mL烧杯中,加入5mL浓硝酸,加热使银完全溶解,稍冷,加入浓盐酸至氯化银沉淀,并至沉淀全部溶解,将烧杯盖上表皿,加热至近干。冷却后,加入2mL王水,用水洗涤,并稀释至约10mL,加热至溶液澄清。冷却后转入25mL比色管中,用水定容。测定结果如下:
1.铜精矿经过上述方法经火试金分离富集后,ICP-AES测定,测定结果与原方法对比结果见表1、表2。结果显示对测定结果没有影响。
表1加银与不加银对金结果的影响:(ICP-AES测定)
编号 | 元素 | 加钯测定结果,g/t | 加银测定金结果,g/t |
18300 | Au | 4.76 | 4.74 |
00064 | Au | 9.18 | 8.90 |
00280 | Au | 3.80 | 3.89 |
00410 | Au | 4.01 | 4.44 |
表2ICP-AES法与原子吸收法测定银结果对照
样品编号 | 元素 | 本方法,g/t | 原子吸收法,g/t |
19-7-0268 | Ag | 478 | 484 |
19-7-0270 | Ag | 73 | 70 |
19-7-0271 | Ag | 151 | 149 |
19-7-0280 | Ag | 483 | 484 |
19-7-0281 | Ag | 24 | 23 |
19-7-0282 | Ag | 66 | 66 |
19-7-0283 | Ag | 150 | 149 |
2.针对银与金的比例小于3时,硝酸很难将银从合粒中完全溶解出来,可能会影响金的王水溶解,选择几乎不含金和银的铜精矿,分别加入不同量的银和金,使银与金质量比为2以下,并加入钯标准溶液1mg/mL两滴(100μg钯)进行实验,结果见表3。
表3加标回收结果
3.选择铜精矿质控样,称取15g数份,在配料中加入钯标准溶液(1g/L)2~4滴。结果表明,银的平行样测定结果十分满意,说明合粒中增加的钯量,在溶解液测定后扣除的措施是合理的,加入不同钯量对银的测定结果没有影响,结果见表4。
表4精密度结果
以上所述的实施例仅是对本发明的优选方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。
Claims (6)
1.一种铜精矿中金银的测定方法,其特征在于:包括以下步骤:
(1)在铜精矿中加入钯标准溶液,得到银合粒;
(2)将银合粒加入到冰乙酸中加热,捞出清洗,烘干;
(3)将银合粒加入到浓硝酸中,加热溶解后,再加入浓盐酸直至沉淀完全溶解,加热蒸干;
(4)加入王水,加热至溶液澄清,冷却后定容,测量金银。
2.根据权利要求1所述的一种铜精矿中金银的测定方法,其特征在于:所述钯标准溶液的浓度为0.8g/L~2g/L。
3.根据权利要求1所述的一种铜精矿中金银的测定方法,其特征在于:所述金铜矿与钯标准溶液的用量比为75000:1~37500:1。
4.根据权利要求1所述的一种铜精矿中金银的测定方法,其特征在于:冰乙酸的用量为15~25mL。
5.根据权利要求1所述的一种铜精矿中金银的测定方法,其特征在于:浓硝酸的用量为5~10mL。
6.根据权利要求1所述的一种铜精矿中金银的测定方法,其特征在于:王水的用量为2~5mL。
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