CN104807949A - Determination method for total sulfur in water quality - Google Patents

Determination method for total sulfur in water quality Download PDF

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CN104807949A
CN104807949A CN201510263305.6A CN201510263305A CN104807949A CN 104807949 A CN104807949 A CN 104807949A CN 201510263305 A CN201510263305 A CN 201510263305A CN 104807949 A CN104807949 A CN 104807949A
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sulfur
water
water quality
total sulfur
water sample
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CN104807949B (en
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张灵芝
杨凤萍
降向正
兰馨辉
葛仲义
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Changchun Gold Research Institute
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Changchun Gold Research Institute
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Abstract

The invention discloses a determination method for total sulfur in water quality. The method includes the following four steps: while sulfurous gas which can leak out is fixed by calcium oxide, potassium permanganate oxidation, nitric acid oxidation, hydrochloric acid regulation and barium chromate spectrophotometry are used for determining sulfate radical, which is converted into sulfur content. During total sulfur determination in water sample, calcium oxide and potassium permanganate are first added to oxidate sulfide ions under alkaline condition, sulfur in other valence states is then oxidated or decomposed into the sulfate radical under the joint oxidation of potassium permanganate and nitric acid, hydrochloric acid solution is then added to regulate the water sample and remove the color of the potassium permanganate, finally, the sulfate radical content in water quality is determined by barium chromate spectrophotometry, and total sulfur content is worked out. According to the characteristics of the sulfur in different valence states in water quality, by fixation, oxidation and decomposition, the method finally converts the sulfur in all valence states into the sulfate radical, and utilizes barium chromate spectrophotometry to determine the sulfate radical, and thereby the total sulfur in water quality is determined. Determination is simple, the result is accurate, and the method can be applied in fields such as environment protection and monitoring, food monitoring and sulfur balance analysis.

Description

The assay method of total sulfur in a kind of water quality
Technical field
The present invention relates to the assay method of total sulfur in the field water quality such as environmental impact assessment, environmental protection, research and application, food, particularly the assay method of total sulfur in a kind of environment monitoring water quality.
Background technology
In surroundings observation process; thiosulfate anion, sulfide, sulfate radical etc. are had in the detection method of the sulphur in water quality; but do not relate to the detection of some other forms of sulphur, to persulfate, the mensuration of the valence state of some sulphur such as sulphite is not easy to.When doing material balance, the balance of sulphur is difficult to do; In environmental issue, in water quality, sulphur is converted into gaseous state and solid-state concrete value is difficult to determine.Therefore, the assay method of total sulfur in a kind of water quality is invented to MaterialBalance Computation, to environmental monitoring, all there is important meaning to food etc.
Summary of the invention
The object of patent of the present invention is exactly the problems referred to above existed for sulphur monitoring, provides the assay method of total sulfur in a kind of water quality.Patent of the present invention is according to the heterogeneity of the sulphur of different valence state, with the sulphur of potassium permanganate and the common oxidizing lower state of nitric acid, and add calcium oxide simultaneously issuable gaseous sulfur is fixed as precipitate morphology, finally be converted into sulfate radical form, add hydrochloric acid heating again and boil several tens minutes, then adopt the sulfate in Barium Chromate Spectrophotometry mensuration water quality.
Step of the present invention is as follows:
(1), appropriate water sample is got, adding distil water is to 50mL, in water sample, add calcium oxide to size mixing supernatant, add liquor potassic permanganate, be alkalescence with sodium hydrate regulator solution pH to solution, heat on electric hot plate, keep micro-heating 15min that boils, if a small amount of potassium permanganate maintenance lavender is added in purple disappearance in heating process;
(2), with distilled water supplement volume of water sample, in water sample, add salpeter solution, keep slight boiling condition heating 10min;
(3), with distilled water supplement volume of water sample, in water sample, add hydrochloric acid solution heating 5min;
(4), take off after to measure sulfate radical in water sample according to Barium Chromate Spectrophotometry, be scaled sulfur content.
In described step (1), when in water quality during sulfur-bearing height, get suitable water sample after can diluting, institute's water sampling sulfur-bearing is not more than 3.3mg.
In described step (1), add calcium oxide supernatant liquid measure of sizing mixing and be not more than 0.8mL, otherwise the calcium oxide needing to do respective volume is omnidistance blank; The liquor potassic permanganate added is the liquor potassic permanganate of mass percent concentration 0.4%, and once adding volume can not be too large, otherwise affects colorimetric; PH scope is regulated to be 7.5 ~ 9.
In described step (2), supplement volume of water sample to about 50mL with distilled water; The salpeter solution added is red fuming nitric acid (RFNA), and volume is 0.5 ~ 2mL; Keep micro-heating 15min that boils, if there is not brown flocculent deposit, can the proper extension heat time.
In described step (3), supplement volume of water sample to about 50mL with distilled water; The hydrochloric acid solution added in water sample is concentration is that 2.5moL/L dilute hydrochloric acid solution is about the micro-heating 5min that boils of 1mL, if brown layering is not fine, and can the proper extension heat time.
In described step (4), sulfate radical in chromate water by Spectrophotometry matter, concrete operation step is for adding the micro-heating 5min that boils of barium chromate suspension, taking off rear ammoniacal liquor, to be adjusted to solution be lemon yellow, many droppings 1 to 2, use Filter paper filtering constant volume at a slow speed in 50mL volumetric flask, to measure absorbance with under 420nm wavelength, contrast with typical curve, calculate sulfur content.
Beneficial effect of the present invention:
The present invention is according to the heterogeneity of sulfocompound in water, with the sulphur of potassium permanganate and the common oxidizing lower state of nitric acid, and add calcium oxide simultaneously issuable gaseous sulfur is fixed as precipitate morphology, and utilized the sulphur heating of high-valence state easily to decompose, finally be converted into sulfate radical form, add hydrochloric acid heating again and boil several tens minutes, then adopt the sulfate in Barium Chromate Spectrophotometry mensuration water quality.
Embodiment
The present invention includes following steps:
(1) (institute's water sampling sulfur-bearing is not more than 3.3mg to get appropriate water sample, suitable water sample is got) after water sample sulfur-bearing height can dilute, adding distil water is to 50mL, in water sample, add calcium oxide to size mixing supernatant, add liquor potassic permanganate, be alkalescence with sodium hydrate regulator solution pH to solution, heat on electric hot plate, keep micro-heating 15min that boils, if a small amount of potassium permanganate maintenance lavender is added in purple disappearance in heating process.
(2) supplement volume of water sample with distilled water, in water sample, add salpeter solution, keep slight boiling condition heating 10min;
(3) supplement volume of water sample with distilled water, in water sample, add hydrochloric acid solution heating 5min.
(4) measure the sulfate radical in water sample according to Barium Chromate Spectrophotometry after taking off, be scaled sulfur content.
In described step (1), when in water quality during sulfur content height, get suitable water sample after can diluting, institute's water sampling sulfur-bearing is not more than 3.3mg.
In described step (1), add calcium oxide supernatant liquid measure of sizing mixing and be not more than 0.8mL, otherwise the calcium oxide needing to do respective volume is omnidistance blank; The liquor potassic permanganate added is the liquor potassic permanganate of mass percent concentration 0.4%, and once adding volume can not be too large, otherwise affects colorimetric; PH scope is regulated to be 7.5 ~ 9.
In described step (2), supplement volume of water sample to about 50mL with distilled water; The salpeter solution added is red fuming nitric acid (RFNA), and volume is 0.5 ~ 2mL; Keep micro-heating 15min that boils, if there is not brown flocculent deposit, can the proper extension heat time.
In described step (3), supplement volume of water sample to about 50mL with distilled water; The hydrochloric acid solution added in water sample is concentration is that 2.5moL/L dilute hydrochloric acid solution is about the micro-heating 5min that boils of 1mL, if brown layering is not fine, and can the proper extension heat time.
In described step (4), sulfate radical in chromate water by Spectrophotometry matter, concrete operation step is for adding the micro-heating 5min that boils of barium chromate suspension, taking off rear ammoniacal liquor, to be adjusted to solution be lemon yellow, many droppings 1 to 2, use Filter paper filtering constant volume at a slow speed in 50mL volumetric flask, to measure absorbance with under 420nm wavelength, contrast with typical curve, calculate sulfur content.
Instantiation 1:
The sulfur-bearing water sample that a kind of sulfur speciation of configuration sulf onyl compound exists, sulfide sulfur-bearing 1mg/mL, gets 2mL water sample and measures according to the method described above, measures sulfate radical result is 6.24mg, and being scaled sulfur content is 2.08mg, and sulfur recovery rate is 104%;
Instantiation 2:
The sulfur-bearing water sample that a kind of sulfur speciation of configuration sulf onyl thiosulfate exists, water sample sulfur-bearing 1mg/mL, gets 2mL water sample and measures according to the method described above, measures sulfate radical result is 6.04mg, and being scaled sulfur content is 2.01mg, and sulfur recovery rate is 101%;
Instantiation 3:
Configuration is only containing the sulfur-bearing water sample that a kind of sulfur speciation of sulphite exists, and water sample sulfur-bearing 1mg/mL, gets 2mL water sample and measure according to the method described above, measures sulfate radical result is 5.84mg, and being scaled sulfur content is 1.95mg, and sulfur recovery rate is 97.5%;
Instantiation 4:
Configuration is only containing the sulfur-bearing water sample that a kind of sulfur speciation of persulfate exists, water sample sulfur-bearing 1mg/mL, gets 2mL water sample and measure according to the method described above, measures sulfate radical result is 6.34mg, and being scaled sulfur content is 2.12mg, and sulfur recovery is 106%;
Instantiation 5:
Configuration is containing the sulfur-bearing water sample of multiple pricing sulphur: get respectively the sulfur compound of above-mentioned configuration, thiosulfate, sulphite, persulfate an aqueous solution 0.5mL, then sampling amount sulfur-bearing total amount is 2mg.Measure according to the method described above, measure sulfate radical result is 6.15mg, being scaled sulfur content is 2.05mg, and sulfur recovery is 103%.

Claims (10)

1. the assay method of total sulfur in water quality, the step of the method is as follows:
(1) appropriate water sample adding distil water, is got to 50mL, in water sample, add calcium oxide to size mixing supernatant, add liquor potassic permanganate, be alkalescence with sodium hydrate regulator solution pH to solution, heat on electric hot plate, keep micro-heating 15min that boils, if a small amount of potassium permanganate maintenance lavender is added in purple disappearance in heating process;
(2), with distilled water supplement volume of water sample, in water sample, add salpeter solution, keep slight boiling condition heating 10min;
(3), with distilled water supplement volume of water sample, in water sample, add hydrochloric acid solution heating 5min;
(4), take off after to measure sulfate radical in water sample according to Barium Chromate Spectrophotometry, be scaled sulfur content.
2. the assay method of total sulfur in a kind of water quality according to claim 1, is characterized in that: in described step (1), adds calcium oxide supernatant liquid measure of sizing mixing and is not more than 0.8mL, otherwise the calcium oxide needing to do respective volume is omnidistance blank.
3. the assay method of total sulfur in a kind of water quality according to claim 1, it is characterized in that: in described step (1), the liquor potassic permanganate added is the liquor potassic permanganate of mass percent concentration 0.4%.
4. the assay method of total sulfur in a kind of water quality according to claim 1, is characterized in that: in described step (1), regulates pH scope to be 7.5 ~ 9.
5. the assay method of total sulfur in a kind of water quality according to claim 1, is characterized in that: in described step (2), supplement volume of water sample to about 50mL with distilled water.
6. the assay method of total sulfur in a kind of water quality according to claim 1, it is characterized in that: in described step (2), the salpeter solution added is red fuming nitric acid (RFNA), and volume is 0.5 ~ 2mL.
7. the assay method of total sulfur in a kind of water quality according to claim 1, is characterized in that: in described step (2), keeps micro-heating 15min that boils, if there is not brown flocculent deposit, and can the proper extension heat time.
8. the assay method of total sulfur in a kind of water quality according to claim 1, is characterized in that: in described step (3), supplement volume of water sample to about 50mL with distilled water.
9. the assay method of total sulfur in a kind of water quality according to claim 1, it is characterized in that: in described step (3), the hydrochloric acid solution added in water sample is concentration is that 2.5moL/L dilute hydrochloric acid solution is about the micro-heating 5min that boils of 1mL, if brown layering is not fine, can the proper extension heat time.
10. the assay method of total sulfur in a kind of water quality according to claim 1, is characterized in that: in described step (1), and when in water quality during sulfur-bearing height, get suitable water sample after can diluting, institute's water sampling sulfur-bearing is not more than 3.3mg.
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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN105527238A (en) * 2015-12-29 2016-04-27 瓮福达州化工有限责任公司 A low-content sulfate radical detecting method for phosphoric acid purified by an industrial wet process
CN106885871A (en) * 2015-12-15 2017-06-23 北京有色金属研究总院 A kind of assay method of complicated solution middle and high concentration sulfate radical
CN107525802A (en) * 2017-07-31 2017-12-29 成都中建材光电材料有限公司 The detection method of sulfur content in a kind of selenium sample
CN107589036A (en) * 2017-07-17 2018-01-16 贵州金洋检测工程有限公司 Test methods of sulphur contents in a kind of water quality
CN108956494A (en) * 2018-06-28 2018-12-07 中国铝业股份有限公司 A kind of method of sulfate radical content in quick measurement bauxite
CN110927003A (en) * 2019-11-14 2020-03-27 徐州伟天化工有限公司 Method for detecting total sulfur in water
CN119780078A (en) * 2025-03-07 2025-04-08 广东环凯生物技术有限公司 Water quality sulfate detection reagent and preparation method thereof, water quality sulfate detection method

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CN102998274A (en) * 2012-11-30 2013-03-27 华南理工大学 Method for rapidly measuring total sulfur content in black pulping liquor
CN103389332A (en) * 2013-07-26 2013-11-13 江苏东华分析仪器有限公司 Electrolytic tank for determining total content of sulphur by adopting microcoulometric method

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106885871A (en) * 2015-12-15 2017-06-23 北京有色金属研究总院 A kind of assay method of complicated solution middle and high concentration sulfate radical
CN105527238A (en) * 2015-12-29 2016-04-27 瓮福达州化工有限责任公司 A low-content sulfate radical detecting method for phosphoric acid purified by an industrial wet process
CN107589036A (en) * 2017-07-17 2018-01-16 贵州金洋检测工程有限公司 Test methods of sulphur contents in a kind of water quality
CN107525802A (en) * 2017-07-31 2017-12-29 成都中建材光电材料有限公司 The detection method of sulfur content in a kind of selenium sample
CN108956494A (en) * 2018-06-28 2018-12-07 中国铝业股份有限公司 A kind of method of sulfate radical content in quick measurement bauxite
CN110927003A (en) * 2019-11-14 2020-03-27 徐州伟天化工有限公司 Method for detecting total sulfur in water
CN119780078A (en) * 2025-03-07 2025-04-08 广东环凯生物技术有限公司 Water quality sulfate detection reagent and preparation method thereof, water quality sulfate detection method

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