CN111537498A - 高氯高盐废水中低浓度重金属元素的测定方法 - Google Patents
高氯高盐废水中低浓度重金属元素的测定方法 Download PDFInfo
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- CN111537498A CN111537498A CN202010404403.8A CN202010404403A CN111537498A CN 111537498 A CN111537498 A CN 111537498A CN 202010404403 A CN202010404403 A CN 202010404403A CN 111537498 A CN111537498 A CN 111537498A
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- 239000000460 chlorine Substances 0.000 title claims abstract description 45
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 43
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 42
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 61
- 239000000243 solution Substances 0.000 claims abstract description 54
- 239000003480 eluent Substances 0.000 claims abstract description 19
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000001632 sodium acetate Substances 0.000 claims abstract description 15
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 15
- 239000012086 standard solution Substances 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 13
- 230000029087 digestion Effects 0.000 claims abstract description 13
- 238000001228 spectrum Methods 0.000 claims abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 34
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 30
- 229910017604 nitric acid Inorganic materials 0.000 claims description 30
- 238000001514 detection method Methods 0.000 claims description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 23
- 239000011780 sodium chloride Substances 0.000 claims description 17
- 239000010949 copper Substances 0.000 claims description 15
- 239000011133 lead Substances 0.000 claims description 15
- 238000010828 elution Methods 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 13
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 11
- 229910052793 cadmium Inorganic materials 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 11
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 10
- 239000005695 Ammonium acetate Substances 0.000 claims description 10
- 229940043376 ammonium acetate Drugs 0.000 claims description 10
- 235000019257 ammonium acetate Nutrition 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 8
- 229910052725 zinc Inorganic materials 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229920001429 chelating resin Polymers 0.000 claims description 4
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 claims description 4
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 239000007853 buffer solution Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 6
- 239000000523 sample Substances 0.000 description 44
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 12
- 238000011084 recovery Methods 0.000 description 10
- 238000004611 spectroscopical analysis Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- 235000019270 ammonium chloride Nutrition 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000007974 sodium acetate buffer Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 229910052745 lead Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012421 spiking Methods 0.000 description 3
- 229910002975 Cd Pb Inorganic materials 0.000 description 2
- 229910017518 Cu Zn Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000002133 sample digestion Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- -1 ammonium ions Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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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- 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
- G01N1/34—Purifying; Cleaning
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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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Plasma & Fusion (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
序号 | 步骤 | 试剂/样品 | 体积 |
1 | 柱活化 | 乙酸铵溶液 | 5ml |
2 | 样品萃取 | 样品溶液 | 10ml |
3 | 淋洗1 | 乙酸铵溶液 | 5ml |
4 | 淋洗2 | 超纯水 | 10ml |
5 | 洗脱 | 硝酸溶液 | 10ml |
分析元素 | Ni | Cu | Zn | Cd | Pb |
分析质量数 | 60 | 63 | 66 | 111 | 208 |
积分时间(s) | 0.1 | 0.1 | 0.2 | 0.1 | 0.1 |
内标元素和质量数 | 70Ge | 70Ge | 70Ge | 103Rh | 185Re |
序号 | Ni | Cu | Zn | Cd | Pb |
1 | 8.71 | 9.93 | 10.80 | 9.36 | 8.51 |
2 | 8.62 | 9.78 | 10.66 | 9.28 | 8.47 |
平均 | 8.66 | 9.85 | 10.73 | 9.32 | 8.49 |
Claims (9)
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN117250253A (zh) * | 2023-11-14 | 2023-12-19 | 中国计量科学研究院 | 一种生物样品中铁、铜和锌的测定方法 |
Citations (9)
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CN105954265A (zh) * | 2016-07-12 | 2016-09-21 | 湖南永清环保研究院有限责任公司 | 一种高盐废水中微量镍的测定方法 |
US20160312337A1 (en) * | 2015-04-23 | 2016-10-27 | Carnegie Mellon University, A Pennsylvania Non-Profit Corporation | Recovery of Rare Earth Elements by Liquid-Liquid Extraction from Fresh Water to Hypersaline Solutions |
JP2016223836A (ja) * | 2015-05-28 | 2016-12-28 | 王子ホールディングス株式会社 | 高塩試料中の金属の分析方法 |
CN107281780A (zh) * | 2017-06-23 | 2017-10-24 | 广州安诺食品科学技术有限公司 | 用于检测茶叶中残留农药的固相萃取柱和检测方法 |
CN107367472A (zh) * | 2017-06-30 | 2017-11-21 | 益盐堂(应城)健康盐制盐有限公司 | 一种快速灵敏检测食盐中多种元素含量的方法 |
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CN109675343A (zh) * | 2018-12-07 | 2019-04-26 | 天津迪沃特生物电子科技有限公司 | 一种萃取和/或净化的方法及装置 |
CN110658143A (zh) * | 2019-11-05 | 2020-01-07 | 华友新能源科技(衢州)有限公司 | 一种高浓度盐水中痕量铋、镉、铬、铜、铁、铅、锌、镍、钴、锰元素含量的测定方法 |
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2020
- 2020-05-13 CN CN202010404403.8A patent/CN111537498A/zh active Pending
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US20160312337A1 (en) * | 2015-04-23 | 2016-10-27 | Carnegie Mellon University, A Pennsylvania Non-Profit Corporation | Recovery of Rare Earth Elements by Liquid-Liquid Extraction from Fresh Water to Hypersaline Solutions |
JP2016223836A (ja) * | 2015-05-28 | 2016-12-28 | 王子ホールディングス株式会社 | 高塩試料中の金属の分析方法 |
CN105954265A (zh) * | 2016-07-12 | 2016-09-21 | 湖南永清环保研究院有限责任公司 | 一种高盐废水中微量镍的测定方法 |
CN107281780A (zh) * | 2017-06-23 | 2017-10-24 | 广州安诺食品科学技术有限公司 | 用于检测茶叶中残留农药的固相萃取柱和检测方法 |
CN107367472A (zh) * | 2017-06-30 | 2017-11-21 | 益盐堂(应城)健康盐制盐有限公司 | 一种快速灵敏检测食盐中多种元素含量的方法 |
CN107652377A (zh) * | 2017-10-18 | 2018-02-02 | 天津出入境检验检疫局动植物与食品检测中心 | 多官能团修饰的螯合树脂的制备方法 |
CN108732000A (zh) * | 2018-08-31 | 2018-11-02 | 青岛卓建海洋装备科技有限公司 | 一种海水重金属预处理装置 |
CN109675343A (zh) * | 2018-12-07 | 2019-04-26 | 天津迪沃特生物电子科技有限公司 | 一种萃取和/或净化的方法及装置 |
CN110658143A (zh) * | 2019-11-05 | 2020-01-07 | 华友新能源科技(衢州)有限公司 | 一种高浓度盐水中痕量铋、镉、铬、铜、铁、铅、锌、镍、钴、锰元素含量的测定方法 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN117250253A (zh) * | 2023-11-14 | 2023-12-19 | 中国计量科学研究院 | 一种生物样品中铁、铜和锌的测定方法 |
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