JP2020528148A - 多硫化ナトリウムの検出方法 - Google Patents
多硫化ナトリウムの検出方法 Download PDFInfo
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- ammonium salt
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- sodium polysulfide
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- 238000000034 method Methods 0.000 title claims abstract description 50
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000012360 testing method Methods 0.000 claims abstract description 50
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 42
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 34
- 239000002244 precipitate Substances 0.000 claims abstract description 32
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 28
- 239000011593 sulfur Substances 0.000 claims abstract description 28
- 238000004448 titration Methods 0.000 claims abstract description 15
- -1 ammonium ions Chemical class 0.000 claims abstract description 13
- 238000003918 potentiometric titration Methods 0.000 claims abstract description 9
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 14
- 229920001021 polysulfide Polymers 0.000 claims description 13
- 239000005077 polysulfide Substances 0.000 claims description 13
- 150000008117 polysulfides Polymers 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical group [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 8
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 7
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 7
- 235000010265 sodium sulphite Nutrition 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 150000004678 hydrides Chemical class 0.000 claims description 5
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 4
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004445 quantitative analysis Methods 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- LNGNZSMIUVQZOX-UHFFFAOYSA-L disodium;dioxido(sulfanylidene)-$l^{4}-sulfane Chemical compound [Na+].[Na+].[O-]S([O-])=S LNGNZSMIUVQZOX-UHFFFAOYSA-L 0.000 claims description 2
- 229940015043 glyoxal Drugs 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical group O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000000243 solution Substances 0.000 description 48
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 18
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000001514 detection method Methods 0.000 description 12
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 9
- 229910052740 iodine Inorganic materials 0.000 description 9
- 239000011630 iodine Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000004734 Polyphenylene sulfide Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229920000069 polyphenylene sulfide Polymers 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001212 derivatisation Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000008098 formaldehyde solution Substances 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- OIRDBPQYVWXNSJ-UHFFFAOYSA-N methyl trifluoromethansulfonate Chemical compound COS(=O)(=O)C(F)(F)F OIRDBPQYVWXNSJ-UHFFFAOYSA-N 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000008055 phosphate buffer solution Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 239000012022 methylating agents Substances 0.000 description 1
- 230000011987 methylation Effects 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
本願は、2018年1月8日に出願した、出願番号が201810015635.7であり、発明の名称が「多硫化ナトリウムの検出方法」である中国特許出願の優先権を主張し、その全ての内容が参照により本願に援用される。
は、0.5mol/L〜1.5mol/Lである。
を取得する。そのうち、硫酸亜鉛溶液を添加し、残されたS2−を除去するためであり、ホルムアルデヒドを使用し、亜硫酸ナトリウムを保護するためである。これは、ヨウドメトリ法により、亜硫酸ナトリウムもヨウ素を消費するからである。
表では、RSDは相対標準偏差である。
Claims (10)
- 試験対象物にアンモニウム塩試薬を滴加し、前記試験対象物中の多硫化ナトリウムを前記アンモニウム塩と反応させ、電位差滴定法により滴定終点を確定して、硫黄沈殿物を得るステップaと、
前記ステップaで消費された前記アンモニウム塩試薬のアンモニウムイオンのモル量及び前記硫黄沈殿物の質量により、前記試験対象物中の多硫化ナトリウムの含有量を計算するステップbと、
を含むことを特徴とする多硫化ナトリウムの検出方法。 - 前記アンモニウム塩試薬は、塩化アンモニウム、硫酸アンモニウム、硫酸水素アンモニウム、硝酸アンモニウム、炭酸アンモニウム又はリン酸アンモニウムであることを特徴とする、請求項1に記載の多硫化ナトリウムの検出方法。
- 前記ステップbにおいて、硫黄沈殿物の質量は、化学定量分析の方法によって取得されることを特徴とする、請求項1に記載の多硫化ナトリウムの検出方法。
- 前記硫黄沈殿物を亜硫酸ナトリウムと反応させ、チオ硫酸ナトリウム沈殿物を得て、ヨウドメトリ法により硫黄沈殿物の質量を得ることを特徴とする、請求項3に記載の多硫化ナトリウムの検出方法。
-
- 前記アンモニウム塩試薬のアンモニウムイオンのモル濃度は、0.5mol/L〜1.5mol/Lであることを特徴とする、請求項5に記載の多硫化ナトリウムの検出方法。
- 前記ステップaにおいて、保護気体の雰囲気下で、前記試験対象物に前記アンモニウム塩試薬を滴加することを特徴とする、請求項1に記載の多硫化ナトリウムの検出方法。
- 前記ステップaにおいて、前記試験対象物に前記アンモニウム塩試薬を滴加する前に、前記試験対象物のpH値を11±0.5に調整することを特徴とする、請求項1に記載の多硫化ナトリウムの検出方法。
- 前記ステップaにおいて、前記試験対象物に前記アンモニウム塩試薬を滴加する前に、前記試験対象物中の硫化水素化物を除去するステップを含むことを特徴とする、請求項1に記載の多硫化ナトリウムの検出方法。
- 前記試験対象物中の硫化水素化物を除去するステップは、具体的には、前記試験対象物に第一試薬及び第二試薬を順に滴加して、前記第一試薬は、ホルムアルデヒド、アセトアルデヒド及びグリオキサールの少なくとも一種であり、前記第二試薬は、塩酸又は硫酸であることを特徴とする、請求項9に記載の多硫化ナトリウムの検出方法。
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CN201810015635.7A CN108226377B (zh) | 2018-01-08 | 2018-01-08 | 多硫化钠的检测方法 |
CN201810015635.7 | 2018-01-08 | ||
PCT/CN2018/093972 WO2019134355A1 (zh) | 2018-01-08 | 2018-07-02 | 多硫化钠的检测方法 |
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CN109851677B (zh) * | 2019-02-26 | 2022-02-25 | 山东大学 | 一种特异性检测多硫化物的蛋白荧光探针及其制备方法与应用 |
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US3874991A (en) * | 1968-08-23 | 1975-04-01 | Westvaco Corp | Polysulfide impregnation of lignocellulosic materials in a continuous digester |
WO2007006150A1 (en) * | 2005-07-13 | 2007-01-18 | Fpinnovations | Method for quantitative determination of individual polysulphide species in oxidized white liquors by means of raman spectroscopy |
CN103983737B (zh) * | 2014-05-26 | 2016-08-24 | 南昌航空大学 | 一种分析铝合金碱性化铣液中复合型多硫化钠的方法 |
CN107188876B (zh) * | 2017-04-10 | 2019-08-09 | 台州学院 | 一种用于检测多硫化氢的近红外荧光探针的合成及应用 |
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CN108226377B (zh) * | 2018-01-08 | 2019-08-23 | 浙江新和成特种材料有限公司 | 多硫化钠的检测方法 |
CN108218772A (zh) * | 2018-03-23 | 2018-06-29 | 潍坊医学院 | 一种用于检测多硫化氢的荧光探针及其制备方法与专用检测试剂盒 |
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