CN110231247A - The measuring method of total sulfate in water and waste water - Google Patents

The measuring method of total sulfate in water and waste water Download PDF

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Publication number
CN110231247A
CN110231247A CN201910642673.XA CN201910642673A CN110231247A CN 110231247 A CN110231247 A CN 110231247A CN 201910642673 A CN201910642673 A CN 201910642673A CN 110231247 A CN110231247 A CN 110231247A
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precipitating
water
beaker
sulfate
measuring method
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李虹
赵建勇
张越
杨璐
李波
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Inner Mongolia Louis Precision Detection Technology Co Ltd
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Inner Mongolia Louis Precision Detection Technology Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses one kind, the measuring method of total sulfate in water and waste water, its purpose is to provide a kind of measuring method for more quickly, accurately and efficiently measuring total sulfate in water and waste water, the present invention uses chloroazotic acid, hydrofluoric acid dissolution sample, and adjusting solution pH value with ammonium hydroxide (1+1) is 7, barium chloride solution sulfate precipitate radical ion, precipitating is stood overnight, and with quantitative filter paper at a slow speed, adds paper pulp filtering, with cold secondary washing beaker, precipitating is washed.Precipitating is placed in porcelain crucible, is ashed in high temperature furnace, calcination 40 minutes under 800-850 degree, and cooling, weighing is taken out.Constant weight.Calculated result.

Description

The measuring method of total sulfate in water and waste water
2, Disclosure of invention
(1) patent name
The measuring method of total sulfate in water and waste water
(2) technical field
The invention belongs to environmental area, a kind of quantitative analysis skill of total sulfate in gravimetric detemination water and waste water is related to Art.
(3) background technique
The bottom deposit layer of water body can be diffused by the sulfate being discharged into ambient water, due to detesting for sedimentary Oxygen environment conditional decision sulfate reducing bacteria will form certain advantage in this space, and along with sulfate reducing bacteria Metabolic activity SO42-S can be converted into2-, these S2-, a part can be with most metal ions present in sedimentary together shape In the sedimentary for precipitating and being deposited on the bottom of water body at the metal sulfide for being insoluble in water, another part then can Yu Shuizhong have Machine object forms sulfurous organic compound, such as sulfuric acid, endangers specifically, water body excessively receives sulfate to generate following several respects to environment Evil:
1;Accelerate the generation of methyl mercury
If containing a certain amount of mercury, the product S of sulfate reduction in water body2-Then sulphur can be formed in mercury present in water body And mercury complex, and it is further converted to methyl mercury, it, can largely due to the presence in sulfate-reducing process Accelerate the generation of methyl mercury.
2;Cause the necessary minor metallic element missing of water plant
In general, the normal growth of water plant be unable to do without certain minor metallic elements, in water bottom sedimentary sulfate In the case that reduction process is active, the product S of sulfate reduction2-Generation metal sulfide can be combined heavy with most of metal ion It forms sediment, aqueous minimum plant metallic element is caused to lack, the ecological balance of water body will be entirely destroyed.
3;Change the original ecological functions of water body
In the case where water body receives excessive sulfate, the sulfate-reducing process of water body lower layer space will become very Active, product hydrogen sulfide generated has very strong toxicity, and the aquatic animals such as fishes and shrimps is caused to become extinct, and loses water body original Ecological functions.
In recent years in water and waste water total sulfate measurement analysis, mostly use that State Environmental Protection Administration works out " water and Effluent monitoring analysis method ", national standard " the measurement gravimetric method of GB11899-89 water quality sulfate ".It is cumbersome, it influences to divide Analyse the accuracy of result, impact analysis speed.Using platinum crucible, platinum ware is expensive, at high cost.Make its application by Certain limitation present invention more has advantage, on the basis of a large amount of analysis practices, this law is made to have quick, accurate, equipment It is required that feature simple, that analysis cost is low, when the routine analysis especially suitable for minimill laboratory substantially reduces analysis Between, reduce loss, improves accuracy.Production efficiency is improved, reagent consumption is reduced and cost of labor, method is easy to grasp And result precision is high, can promote and apply in production.Simple using equipment, analysis process is short, has accurately and rapidly special Point, the measurement analysis suitable for sulfate in water and waste water.
(4) content
Purpose: it is short to formulate a kind of operating process, at low cost, quickly, efficiently, it is accurate, stability is good, is easy to the measurement grasped The analysis method of sulfate in water and waste water.
Technical solution:
The present invention is to measure the content of sulfate in water and waste water.
Specifically completed by following steps
Chloroazotic acid 10mL, 1-2 drop hydrofluoric acid are used in beaker.Dissolved samples, adjusting solution pH value with ammonium hydroxide (1+1) is 7, (if there is precipitating is filtered with Medium speed filter paper, if do not precipitated without this step) be added barium chloride solution precipitated sulfur acid group from Son, precipitating are stood overnight, and with quantitative filter paper at a slow speed, add paper pulp filtering, are cleaned with cold secondary washing beaker and with wiping stick, are washed precipitating 10 times,
Precipitating is placed in porcelain crucible, is carefully ashed in high temperature furnace, calcination 40 minutes under 800-850 degree, taking-up cooling, Weighing.Constant weight.Calculated result.
(5) beneficial effect
1) quickly, efficiently, low cost: this method substantially reduces operating process, has saved drug, reduce detection at This, improves production efficiency.
2) accurate, stable: to use this method, measurement result is stablized, and data are accurate.
(6) specific embodiment
1. method summary:
Chloroazotic acid 10mL, 1-2 drop hydrofluoric acid are used in beaker.Dissolved samples, adjusting solution pH value with ammonium hydroxide (1+1) is 7, (if there is precipitating is filtered with Medium speed filter paper, if do not precipitated without this step) be added barium chloride solution precipitated sulfur acid group from Son, precipitating are stood overnight, and with quantitative filter paper at a slow speed, add paper pulp filtering, are cleaned with cold secondary washing beaker and with wiping stick, are washed precipitating 10 times,
Precipitating is placed in porcelain crucible, is carefully ashed in high temperature furnace, calcination 40 minutes under 800-850 degree, taking-up cooling, Weighing.Constant weight.Calculated result.
2. reagent:
2.1 chloroazotic acid (+1 part of nitric acid of 3 parts of hydrochloric acid)
2.2 ammonium hydroxide (1+1)
2.3 hydrofluoric acid (40%)
2.4 barium chloride solutions (100g/L)
5. analytical procedure:
Sample 100mL is pipetted in 400mL beaker, 10mL chloroazotic acid, 1-2 drop hydrofluoric acid are added in beaker.Heating is boiled, Dissolved samples dissolve sample all, and heating is boiled, and keep solution 5 minutes, and with ammonium hydroxide (1+1), adjusting solution pH value is 7, (if there is precipitating is filtered with Medium speed filter paper, if do not precipitated without this step).Side stirring, edge wall of cup slowly add Enter, barium chloride solution 20mL is added dropwise, sulfate precipitate radical ion boils 5 minutes, and precipitating is stood overnight, and with quantitative filter paper at a slow speed, is added Paper pulp filtering is cleaned with cold secondary washing beaker and with wiping stick, washes precipitating 10 times,
Precipitating is placed in porcelain crucible, is carefully ashed in high temperature furnace, calcination 40 minutes under 800-850 degree, taking-up cooling, Weighing.Constant weight.Write down m1
Blank;
Secondary water 100mL is pipetted in 400mL beaker, 10mL chloroazotic acid, 1-2 drop hydrofluoric acid are added in beaker.Heating is boiled Boiling, dissolved samples dissolve sample all, and heating is boiled, and keep solution 5 minutes, with ammonium hydroxide (1+1), adjust solution PH Value is 7, (if there is precipitating is filtered with Medium speed filter paper, if do not precipitated without this step).Side stirring, edge wall of cup it is slow It being added, barium chloride solution 20mL is added dropwise, sulfate precipitate radical ion boils 5 minutes, and precipitating is stood overnight, with quantitative filter paper at a slow speed, Add paper pulp filtering, cleaned with cold secondary washing beaker and with wiping stick, washes precipitating 10 times,
Precipitating is placed in porcelain crucible, is carefully ashed in high temperature furnace, calcination 40 minutes, takes under 800-850 degree Muffle furnace Cooling out, weighing.Constant weight.Write down m0
6. Analysis result calculation:
SO4 2-(mg/L)=(m1-m0) × 0.4115 × 1000/V
In formula: m1: the quality (mg) of the barium sulfate precipitated in sample
M0: the quality (mg) of the barium sulfate precipitated in blank
0.4115: barium sulfate weight is scaled SO4 2-Coefficient
V: the volume (mL) pipetted
(7) analysis method compares:
Accuracy:
As can be seen from the above table: resulting data are measured, it is suitable with national standard method, state environmental monitoring analysis method.And Operating process is short, quickly, efficiently.
Precision:
As can be seen from the above table: measuring resulting data, precision is high
(8) conclusion:
By this method, the content that sulfate in waste water is drunk in water outlet can be accurately measured.The operating time is substantially reduced, Reduce energy consumption.So that determination data is accurate and reliable, application obtains preferable effect in production.

Claims (4)

1. the measuring method of total sulfate in water and waste water: including blank;
Secondary water 100mL is pipetted in 400mL beaker, 10mL chloroazotic acid, 1-2 drop hydrofluoric acid are added in beaker.Heating is boiled, molten Sample is solved, dissolves sample all, heating is boiled, and keeps solution 5 minutes, and with ammonium hydroxide (1+1), adjusting solution pH value is 7, (if there is precipitating is filtered with Medium speed filter paper, if do not precipitated without this step).Side stirring, edge wall of cup be slowly added to, Barium chloride solution 20mL is added dropwise, sulfate precipitate radical ion boils 5 minutes, and precipitating is stood overnight, and with quantitative filter paper at a slow speed, adds paper Slurry filtering, is cleaned with cold secondary washing beaker and with wiping stick, washes precipitating 10 times.
2. the measuring method of total sulfate in water as described in claim 1 and waste water.It is characterized by: pipette sample 100mL in In 400mL beaker, 10mL chloroazotic acid, 1-2 drop hydrofluoric acid are added in beaker.Heating is boiled, dissolved samples, keeps sample all molten Solution, heating are boiled, and keep solution 5 minutes, and with ammonium hydroxide (1+1), adjusting solution pH value is 7, (if there is precipitating is filtered with middling speed Paper filtering, if do not precipitated without this step).Side stirring, edge wall of cup be slowly added to, be added dropwise barium chloride solution 20mL, Sulfate precipitate radical ion boils 5 minutes, and precipitating is stood overnight, and with quantitative filter paper at a slow speed, adds paper pulp filtering, with cold secondary washing Beaker is simultaneously cleaned with wiping stick, washes precipitating 10 times.Precipitating is placed in porcelain crucible, is carefully ashed in high temperature furnace, under 800-850 degree Calcination 40 minutes, take out cooling, weighing.Constant weight.Calculated result.
3. such as claim: the measuring method of total sulfate in 2 water and waste water.It is characterized by: chloroazotic acid: 3 parts of hydrochloric acid+1 Part nitric acid, ammonium hydroxide: barium chloride solution (100g/L) :+1 part of secondary water of 1 part of ammonium hydroxide weighs 100g barium chloride in beaker, with two Secondary water dissolves and constant volume is in 1000mL volumetric flask.
4. such as claim: the measuring method of total sulfate in 3 water and waste water.It is characterized by:
Chloroazotic acid 10mL, 1-2 drop hydrofluoric acid are used in beaker.Dissolved samples, adjusting solution pH value with ammonium hydroxide (1+1) is 7, (such as Fruit has precipitating to be filtered with Medium speed filter paper, if do not precipitated without this step) barium chloride solution sulfate precipitate radical ion is added, it sinks Shallow lake is stood overnight, and with quantitative filter paper at a slow speed, adds paper pulp filtering, is cleaned with cold secondary washing beaker and with wiping stick, washes precipitating 10 times,
Precipitating is placed in porcelain crucible, is carefully ashed in high temperature furnace, calcination 40 minutes under 800-850 degree, and cooling, title is taken out Weight.Constant weight.Calculated result.
CN201910642673.XA 2019-07-16 2019-07-16 The measuring method of total sulfate in water and waste water Withdrawn CN110231247A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110864994A (en) * 2019-11-06 2020-03-06 攀枝花钢城集团瑞达水泥有限公司 Method for measuring sulfate sulfur trioxide
CN114062186A (en) * 2020-07-31 2022-02-18 上海梅山钢铁股份有限公司 Method for determining content of calcium sulfate in sintering desulfurization and denitrification ash
CN114112770A (en) * 2021-11-17 2022-03-01 超威电源集团有限公司 Method for detecting uniformity of lead paste of negative electrode of lead-acid storage battery

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103454175A (en) * 2013-08-15 2013-12-18 贵州航天精工制造有限公司 Method for determining niobium content in aeronautical material Ti45Nb titanium alloy
CN104142283A (en) * 2014-08-04 2014-11-12 攀枝花学院 Method for measuring barium titanate content
CN104237059A (en) * 2014-09-25 2014-12-24 武汉钢铁(集团)公司 Determination method of sulfate radical content in chromium plating solution
CN104819908A (en) * 2015-04-29 2015-08-05 内蒙古包钢钢联股份有限公司 Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy
CN105067614A (en) * 2015-08-21 2015-11-18 内蒙古包钢钢联股份有限公司 Method for continuous determination of content of Ca, Mg and Ba in Si-Ca-Ba-Mg alloy
CN106018160A (en) * 2016-06-24 2016-10-12 安徽创新检测技术有限公司 Method for measuring content of water-soluble and acid-soluble sulfate in soil
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103454175A (en) * 2013-08-15 2013-12-18 贵州航天精工制造有限公司 Method for determining niobium content in aeronautical material Ti45Nb titanium alloy
CN104142283A (en) * 2014-08-04 2014-11-12 攀枝花学院 Method for measuring barium titanate content
CN104237059A (en) * 2014-09-25 2014-12-24 武汉钢铁(集团)公司 Determination method of sulfate radical content in chromium plating solution
CN104819908A (en) * 2015-04-29 2015-08-05 内蒙古包钢钢联股份有限公司 Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy
CN105067614A (en) * 2015-08-21 2015-11-18 内蒙古包钢钢联股份有限公司 Method for continuous determination of content of Ca, Mg and Ba in Si-Ca-Ba-Mg alloy
CN106018160A (en) * 2016-06-24 2016-10-12 安徽创新检测技术有限公司 Method for measuring content of water-soluble and acid-soluble sulfate in soil
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

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
吴志义: "《修井工程》", 31 March 1991, 石油工业出版社 *
国家环境保护局: "《GB11899-89水质硫酸盐的测定重量法》", 1 July 1990 *
张毂: "《岩石矿物分析》", 30 April 1992, 地质出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110864994A (en) * 2019-11-06 2020-03-06 攀枝花钢城集团瑞达水泥有限公司 Method for measuring sulfate sulfur trioxide
CN114062186A (en) * 2020-07-31 2022-02-18 上海梅山钢铁股份有限公司 Method for determining content of calcium sulfate in sintering desulfurization and denitrification ash
CN114112770A (en) * 2021-11-17 2022-03-01 超威电源集团有限公司 Method for detecting uniformity of lead paste of negative electrode of lead-acid storage battery

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