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 PDFInfo
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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
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.
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Cited By (3)
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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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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 |
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