CN104807949B - The assay method of total sulfur in a kind of water quality - Google Patents
The assay method of total sulfur in a kind of water quality Download PDFInfo
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- CN104807949B CN104807949B CN201510263305.6A CN201510263305A CN104807949B CN 104807949 B CN104807949 B CN 104807949B CN 201510263305 A CN201510263305 A CN 201510263305A CN 104807949 B CN104807949 B CN 104807949B
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Abstract
The invention discloses the assay method of total sulfur in a kind of water quality, the method is to be measured sulfate radical and be converted into sulfur content with potassium permanganate oxidation, nitric acid oxidation, hydrochloric acid regulation, Barium Chromate Spectrophotometry by the fixing possible excessive sulfurous gas of calcium oxide simultaneously, four steps compositions；In water sample during Determination Method of Total Sulfide Content, it is firstly added calcium oxide and potassium permanganate aoxidizes sulfidion in the basic conditions, under the common oxidation of potassium permanganate and nitric acid, the sulphur of other valence states aoxidized again or be decomposed into sulfate radical, it is subsequently adding hydrochloric acid solution regulation water sample and makes the color of potassium permanganate be removed, measure sulfate radical content in water quality finally by Barium Chromate Spectrophotometry, calculate total sulfur content.The present invention is according to the feature of different valence state sulphur in water quality, and by fixing, aoxidize and decomposing, the sulphur of the most all valence states is converted into sulfate radical, realizes the mensuration of total sulfur in water quality by barium chromate method spectrophotometry sulfate radical.The fields such as this method measures simple, and result is accurate, the permissible sulfur balance analysis being applied in environment monitoring, Food Monitoring, environmental impact assessment.
Description
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 to the assay method of total sulfur in a kind of environment monitoring water quality.
Background technology
Surroundings monitoring during, the detection method of the sulphur in water quality has thiosulfate anion, sulfide,
Sulfate radical etc., but it is not involved with the detection of some other forms of sulphur, to persulfate, sulfurous acid
The mensuration of the valence state of some sulphur such as salt 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 the concrete value of gaseous state and solid-state and is difficult to determine.Therefore,
Invent in a kind of water quality the assay method of total sulfur to MaterialBalance Computation, to environmental monitoring, to food etc. all
There is important meaning.
Summary of the invention
The purpose of patent of the present invention is aiming at the problems referred to above that sulphur monitoring exists, it is provided that total in a kind of water quality
The assay method of sulphur.Patent of the present invention is according to the heterogeneity of the sulphur of different valence state, with potassium permanganate and nitre
The sulphur of the common oxidizing lower state of acid, and be simultaneously introduced calcium oxide issuable gaseous sulfur is fixed as precipitation
Form, is finally converted into sulfate radical form, adds hydrochloric acid heating again and boils several tens minutes, so
Rear employing Barium Chromate Spectrophotometry measures the sulfate in water quality.
The step of the present invention is as follows:
(1), take appropriate water sample, add distilled water to 50mL, in water sample, add calcium oxide size mixing supernatant,
Add liquor potassic permanganate, be alkalescence with sodium hydrate regulator solution pH to solution, add on electric hot plate
Heat, keep micro-boiling heating 15min, if in heating process purple disappear add a small amount of potassium permanganate maintain pale purple
Look；
(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), take off after measure in water sample according to Barium Chromate Spectrophotometry sulfate radical, be scaled sulphur and contain
Amount.
In described step (1), when sulfur-bearing height in water quality, suitable water sample, institute's water sampling after diluting, can be taken
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 need to do
The calcium oxide whole process of respective volume is blank；The liquor potassic permanganate added is mass percent concentration 0.4%
Liquor potassic permanganate, once adding volume can not be too big, otherwise affects colorimetric；Regulation pH scope is 7.5～9.
In described step (2), supplement volume of water sample to about 50mL with distilled water；The nitric acid added is molten
Liquid is red fuming nitric acid (RFNA), and volume is 0.5～2mL；Keep micro-boiling heating 15min, if brown flocculent deposit does not occurs,
Can the proper extension heat time.
In described step (3), supplement volume of water sample to about 50mL with distilled water；Add in water sample
Hydrochloric acid solution be concentration be 2.5moL/L dilute hydrochloric acid solution about 1mL micro-boiling heating 5min, if brown is divided
Layer is not fine, can the proper extension heat time.
In described step (4), sulfate radical in chromate water by Spectrophotometry matter, concrete operation step
For add barium chromate suspension micro-boiling heating 5min, after taking off with ammoniacal liquor regulation to solution be lemon yellow,
Many droppings 1 to 2, with in Filter paper filtering constant volume at a slow speed to 50mL volumetric flask, and under 420nm wavelength
Measure absorbance, contrast with calibration curve, calculate sulfur content.
Beneficial effects of the present invention:
The present invention, according to the heterogeneity of sulfur-containing compound in water, aoxidizes low with potassium permanganate and nitric acid jointly
The sulphur of valence state, and be simultaneously introduced calcium oxide issuable gaseous sulfur is fixed as precipitate morphology, and utilize
The sulphur heating crossing high-valence state is easily decomposed, and is finally converted into sulfate radical form, adds hydrochloric acid again and adds
Heat boils several tens minutes, then uses Barium Chromate Spectrophotometry to measure the sulfate in water quality.
Detailed description of the invention
The present invention comprises the following steps:
(1) (institute's water sampling sulfur-bearing is not more than 3.3mg, and water sample sulfur-bearing height can take after diluting to take appropriate water sample
Suitably water sample), add distilled water to 50mL, in water sample, add calcium oxide size mixing supernatant, addition Gao Meng
Acid potassium solution, is alkalescence with sodium hydrate regulator solution pH to solution, heats on electric hot plate, keeps
Micro-boiling heating 15min, 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 to add
Hot 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 sulfur content height in water quality, suitable water sample can be taken after diluting, fetched water
Sample 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 need to do
The calcium oxide whole process of respective volume is blank；The liquor potassic permanganate added is mass percent concentration 0.4%
Liquor potassic permanganate, once adding volume can not be too big, otherwise affects colorimetric；Regulation pH scope is 7.5～9.
In described step (2), supplement volume of water sample to about 50mL with distilled water；The nitric acid added is molten
Liquid is red fuming nitric acid (RFNA), and volume is 0.5～2mL；Keep micro-boiling heating 15min, if brown flocculent deposit does not occurs,
Can the proper extension heat time.
In described step (3), supplement volume of water sample to about 50mL with distilled water；Add in water sample
Hydrochloric acid solution be concentration be 2.5moL/L dilute hydrochloric acid solution about 1mL micro-boiling heating 5min, if brown is divided
Layer is not fine, can the proper extension heat time.
In described step (4), sulfate radical in chromate water by Spectrophotometry matter, concrete operation step
For add barium chromate suspension micro-boiling heating 5min, after taking off with ammoniacal liquor regulation to solution be lemon yellow,
Many droppings 1 to 2, with in Filter paper filtering constant volume at a slow speed to 50mL volumetric flask, and under 420nm wavelength
Measure absorbance, contrast with calibration curve, calculate sulfur content.
Instantiation 1:
The sulfur-bearing water sample that configuration a kind of sulfur speciation of sulf onyl compound exists, sulfide sulfur-bearing 1mg/mL, take 2mL
Water sample is measured according to the method described above, measure sulfate radical result is 6.24mg, being scaled sulfur content is
2.08mg, sulfur recovery rate is 104%；
Instantiation 2:
The sulfur-bearing water sample that configuration a kind of sulfur speciation of sulf onyl thiosulfate exists, water sample sulfur-bearing 1mg/mL, take 2mL
Water sample is measured according to the method described above, measure sulfate radical result is 6.04mg, being scaled sulfur content is
2.01mg, sulfur recovery rate is 101%；
Instantiation 3:
The sulfur-bearing water sample that configuration only exists containing a kind of sulfur speciation of sulphite, water sample sulfur-bearing 1mg/mL, take 2mL
Water sample is measured according to the method described above, measure sulfate radical result is 5.84mg, being scaled sulfur content is
1.95mg, sulfur recovery rate is 97.5%；
Instantiation 4:
The sulfur-bearing water sample that configuration only exists containing a kind of sulfur speciation of persulfate, water sample sulfur-bearing 1mg/mL, take 2mL
Water sample is measured according to the method described above, measure sulfate radical result is 6.34mg, being scaled sulfur content is
2.12mg, sulfur recovery is 106%；
Instantiation 5:
Configuration is containing the sulfur-bearing water sample of multiple pricing sulphur: take respectively the sulfur compound of above-mentioned configuration, thiosulfate,
Sulphite, persulfate the aqueous solution 0.5mL, then sampling amount sulfur-bearing total amount is 2mg.According to above-mentioned
Method is measured, measure sulfate radical result is 6.15mg, being scaled sulfur content is 2.05mg, sulfur recovery
It is 103%.
Claims (5)
1. an assay method for total sulfur in water quality, the step of the method is as follows:
(1), take appropriate water sample and add distilled water to 50mL, in water sample, add calcium oxide size mixing supernatant,
Add liquor potassic permanganate, be alkalescence with sodium hydrate regulator solution pH to solution, add on electric hot plate
Heat, keep micro-boiling heating 15min, if in heating process purple disappear add a small amount of potassium permanganate maintain pale purple
Look；
(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), take off after measure in water sample according to Barium Chromate Spectrophotometry sulfate radical, be scaled sulphur and contain
Amount；
In described step (1), add calcium oxide supernatant liquid measure of sizing mixing and be not more than 0.8mL；
In described step (1), the liquor potassic permanganate of addition is the permanganic acid of mass percent concentration 0.4%
Potassium solution；
In described step (3), in water sample add hydrochloric acid solution be concentration be 2.5moL/L watery hydrochloric acid
Solution 1mL, micro-boiling heating 5min.
The assay method of total sulfur in a kind of water quality the most according to claim 1, it is characterised in that: institute
Stating in step (1), regulation pH scope is 7.5～9.
The assay method of total sulfur in a kind of water quality the most according to claim 1, it is characterised in that: institute
State in step (2), supplement volume of water sample to about 50mL with distilled water.
The assay method of total sulfur in a kind of water quality the most according to claim 1, it is characterised in that: institute
State in step (3), supplement volume of water sample to about 50mL with distilled water.
The assay method of total sulfur in a kind of water quality the most according to claim 1, it is characterised in that: institute
Stating in step (1), when sulfur-bearing height in water quality, can take suitable water sample after diluting, institute's water sampling sulfur-bearing is not
More than 3.3mg.
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| 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 |
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| US5152963A (en) * | 1986-08-04 | 1992-10-06 | Wreyford Donald M | Total sulfur analyzer system operative on sulfur/nitrogen mixtures |
| CN1191473C (en) * | 2000-03-03 | 2005-03-02 | 中国石油化工集团公司 | Method for measuring total active sulfur in petroleum fractions |
| US6830730B2 (en) * | 2001-09-11 | 2004-12-14 | Spectrolanalytical Instruments | Method and apparatus for the on-stream analysis of total sulfur and/or nitrogen in petroleum products |
| JP4948380B2 (en) * | 2007-12-20 | 2012-06-06 | 東京電力株式会社 | Method for determination of sulfonic acid type sulfur content in insulating oil |
| 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 |
| CN103389332B (en) * | 2013-07-26 | 2016-04-27 | 江苏东华分析仪器有限公司 | Total sulfur content micro-coulometric determination electrolytic cell |
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