CN106865503A - A kind of method of micro total nitrogen and ammonia nitrogen in removal potassium peroxydisulfate - Google Patents
A kind of method of micro total nitrogen and ammonia nitrogen in removal potassium peroxydisulfate Download PDFInfo
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- CN106865503A CN106865503A CN201710152018.7A CN201710152018A CN106865503A CN 106865503 A CN106865503 A CN 106865503A CN 201710152018 A CN201710152018 A CN 201710152018A CN 106865503 A CN106865503 A CN 106865503A
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- potassium peroxydisulfate
- total nitrogen
- nitrogen
- ammonia nitrogen
- potassium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
- C01B15/06—Peroxyhydrates; Peroxyacids or salts thereof containing sulfur
- C01B15/08—Peroxysulfates
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Abstract
The invention belongs to technical field of analytical chemistry, a kind of method for removing micro total nitrogen and ammonia nitrogen in potassium peroxydisulfate is disclosed.Methods described is：Pure water is heated to 50 DEG C of insulations, it is subsequently adding potassium peroxydisulfate stirring and dissolving to saturation state, crystallized as at a temperature of 4 DEG C after gained saturation potassium persulfate solution is sealed, taken out when crystal is no longer separated out, abandoning supernatant, crystal is cleaned with 4 DEG C of pure water, is then dried at a temperature of 50 DEG C, obtain removing the potassium peroxydisulfate after micro total nitrogen and ammonia nitrogen.The inventive method is simple to operate, and the removal effect of total nitrogen and ammonia nitrogen is good, and the rate of recovery of potassium peroxydisulfate product is high, and the quality requirement of the total nitrogen analysis of low concentration is satisfied with after purifying products.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to micro total nitrogen and ammonia nitrogen in a kind of removal potassium peroxydisulfate
Method.
Background technology
Potassium peroxydisulfate be it is a kind of basis, using extensive chemical reagent, under some service conditions, such as be used for total nitrogen
Determine, be have strict demand for its quality.Total nitrogen index is to characterize sewage and the most basic water quality of surface water body environmental quality
One of parameter, is also the important parameter for weighing Eutrophic Extent, determines very high frequency,《The measure alkalescence over cure of water quality total nitrogen
Sour potassium ultraviolet spectrophotometry》(HJ 636-2012) is because its is easy to operate, instrument popularity rate high, sensitivity and good stability
The features such as, thus the measure of total nitrogen uses the method substantially.But, domestic potassium peroxydisulfate refers to as strong oxidizer for water quality
When marking the measure of total nitrogen, often occur making blank value too high because of the addition of potassium peroxydisulfate, so as to cause standard curve linearly poor
The problems such as, the degree of accuracy and the precision of total nitrogen data are influenceed, even cannot set up effective standard curve during most serious.It is of the invention special
The previous work of profit shows that this is too high closely bound up with total nitrogen in domestic potassium peroxydisulfate and ammonia-nitrogen content.Although, for persulfuric acid
The total nitrogen content of potassium has relevant criterion to be specified, such as：《The measure alkaline chitinase ultraviolet spectrophotometry of water quality total nitrogen》
Quality requirement in (HJ 636-2012) to total nitrogen content in potassium peroxydisulfate is：TN≤0.005%；The life of domestic potassium peroxydisulfate
Product is performed both by《Chemical reagent potassium persulfate (potassium peroxydisulfate)》(GB/T 641-2011), the standard to potassium peroxydisulfate in it is total
The quality requirement of nitrogen content is：TN≤0.0005%；But the manufacturer of the country is substantially all and fails to meet above-mentioned requirements, this
Also so that produced problem cannot be solved in total nitrogen index determining at all.
In order to solve the above problems, each laboratory and monitoring station are frequently with two ways：(1) external production is directly bought
Potassium peroxydisulfate reagent, its quality can meet measure demand, but costly, and by taking 500g/ bottles of potassium peroxydisulfate as an example, Sigma is public
The price of both department and Chinese medicines group is respectively 1014 yuan and 31 yuan, and the former is nearly 33 times of the latter；(2) in laboratory to domestic
Potassium peroxydisulfate carries out repeated recrystallize purification, meets measure demand and reuses.But, often by measure after recrystallization operation
Whether its blank value is weighed less than limit value 0.03 specified in standard method, although the method is simple to operate, but wherein people
Power cost and time cost are easily ignored, and time-consuming, the rate of recovery is low.
Patent of invention (publication number CN104176748A) is referred to a kind of method of purification of potassium peroxydisulfate, but the method is present
Following three major issue：(1) operation temperature is set as 40 DEG C, the first time rate of recovery of potassium peroxydisulfate less than 50%, three weights
The rate of recovery after crystallization is even more as little as less than 12.5%, and the rate of recovery of potassium peroxydisulfate is low, uneconomical；(2) the method is used
Alkaline chitinase is, it is necessary to additionally add NaOH, production cost is high；(3) mechanism of purification potassium peroxydisulfate is indefinite, only
By personal experience.
The content of the invention
In order to solve the shortcoming and defect part of above prior art, it is an object of the invention to provide one kind removal over cure
The method of micro total nitrogen in sour potassium.
The object of the invention is achieved through the following technical solutions：
The method of micro total nitrogen and ammonia nitrogen, comprises the following steps in a kind of removal potassium peroxydisulfate：
Pure water is heated to 50 DEG C of insulations, potassium peroxydisulfate stirring and dissolving to saturation state is subsequently adding, by gained saturation mistake
Crystallized as at a temperature of 4 DEG C after potassium sulfate solution sealing, taken out when crystal is no longer separated out, abandoning supernatant is clear with 4 DEG C of pure water
Crystal is washed, is then dried at a temperature of 50 DEG C, obtain removing the potassium peroxydisulfate after micro total nitrogen and ammonia nitrogen.
Preferably, the number of times that crystal is cleaned with 4 DEG C of pure water is 3 times.
The method of the present invention has the following advantages that and beneficial effect：
(1) the inventive method is simple to operate, and the removal effect of total nitrogen and ammonia nitrogen is good, and the rate of recovery of potassium peroxydisulfate product is high,
And the quality requirement of the total nitrogen analysis of low concentration is satisfied with after purifying products；
(2) temperature of the inventive method dissolving potassium peroxydisulfate is 50 DEG C, it is ensured that the rate of recovery of recrystallization keeps for the first time
To more than 75%, the rate of recovery after second rate of recovery of recrystallization is more than 50%, and third time is recrystallized for 41% with
On, the rate of recovery of potassium peroxydisulfate is high, and actual application value is high；
(3) crystallization temperature of the inventive method potassium peroxydisulfate is 4 DEG C, and cleans crystal with 4 DEG C of pure water, can effectively be ensured
The yield of potassium peroxydisulfate and effectively removal are attached to the micro nitrogen material on crystal；
(4) drying temperature of potassium persulfate crystals is 50 DEG C in the inventive method, is ensureing potassium peroxydisulfate not because of high temperature point
While solution, rate of drying is improved, so as to improve the efficiency of whole removal process.
Brief description of the drawings
Under Fig. 1 is for different recrystallization times conditions, total nitrogen quality is divided in four kinds of potassium peroxydisulfates (label 1#, 2#, 3# and 4#)
Several variation diagrams；
Under Fig. 2 is for different recrystallization times conditions, ammonia nitrogen quality is divided in four kinds of potassium peroxydisulfates (label 1#, 2#, 3# and 4#)
Several variation diagrams；
Fig. 3 is recrystallized under times conditions for different, four kinds of domestic potassium peroxydisulfate (good fortune morning, great Mao, Aladdin, traditional Chinese medicines) blank
The variation diagram of value；
Fig. 4 is that potassium peroxydisulfate carries out the dynamic analysis curve map of total nitrogen removal in the inventive method.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.
Embodiment
Four kinds of potassium peroxydisulfates (label 1#, 2#, 3# and 4#) are carried out into recrystallization removal total nitrogen and ammonia nitrogen：
(1) measure in 800mL pure water to 1000mL beakers, heated in 50 DEG C of water-baths, rallentando add over cure
Sour potassium product (about 130g or so), and be stirred continuously with glass bar, when beaker bottom has a small amount of solid not to be redissolved, stop stirring
Mix and take out；
(2) rapid beaker mouthful is strictly sealed with PE films, it is quiet that beaker and solution therein are transferred into 4 DEG C of refrigerators
Put, the extraneous factor interference such as do not allow solution vibrated in the process is taken out when crystal is no longer separated out；
(3) supernatant of crystallization is discarded, the crystal of precipitation 4 DEG C of pure water rinsings 3 times, then crystal is transferred to 250mL
In beaker；
(4) crystal is put into 50 DEG C of baking ovens and is dried, rear taking-up to be dried；
(5) measure in 600mL pure water to 1000mL beakers, heated in 50 DEG C of water-baths, rallentando add step
(4) the potassium peroxydisulfate reagent (about 105g or so) obtained by drying, and be stirred continuously with glass bar, when beaker bottom has a small amount of solid
When not being redissolved, stopping is stirred and taken out；Repeat step (2), (3), (4)；
(6) measure in 450mL pure water to 1000mL beakers, heated in 50 DEG C of water-baths, rallentando add step
(5) the potassium peroxydisulfate reagent (about 80g or so) obtained by drying, and be stirred continuously with glass bar, when beaker bottom has a small amount of solid
When not being redissolved, stopping is stirred and taken out；Repeat step (2), (3), (4)；
(7) crystal obtained by step (6) is put into wide-mouth Brown Glass Brown glass bottles and jars only, sealing preserve.
Under difference recrystallization times condition, the change of total nitrogen content in four kinds of potassium peroxydisulfates (label 1#, 2#, 3# and 4#)
Change and HJ636-2012 and GB/T 641-2011 normal lines are as shown in Figure 1；Under difference recrystallization times condition, four kinds of persulfuric acid
The change of ammonia nitrogen mass fraction is as shown in Figure 2 in potassium (label 1#, 2#, 3# and 4#)；Under difference recrystallization times condition, four kinds of states
The situation of change and HJ636-2012 normal lines for producing potassium peroxydisulfate (good fortune morning, great Mao, Aladdin, traditional Chinese medicines) blank value are as shown in Figure 3.
The removal efficiency that can be seen that total nitrogen and ammonia nitrogen by the result of Fig. 1~3 is all very high.Total nitrogen and ammonia nitrogen after recrystallizing for the first time
Removal efficiency is up to 95.6% and 98.1% respectively.After recrystallization 2 times, the product quality of above-mentioned four kinds of potassium peroxydisulfates is satisfied by
The requirement of HJ636-2012, while the blank value of potassium peroxydisulfate also reaches the requirement less than 0.03.The potassium peroxydisulfate of the present embodiment
Recrystallize for the first time, the rate of recovery of second recrystallization and third time recrystallization is respectively 75%~77%, 50%~58%, with
And 41%~43%.
The dynamic analysis of total nitrogen removal is carried out to four kinds of potassium peroxydisulfates of the present embodiment (label 1#, 2#, 3# and 4#), as a result
As shown in Fig. 4 (by taking 1# as an example), the removal process of total nitrogen meets first order exponential decay equation (Y=A × e-Bt+ C, R2=
0.99999).With reference to first-order exponential decay fitting parameter, can be to the total nitrogen removal of potassium peroxydisulfate under different recrystallization times conditions
Efficiency is estimated.
Four kinds of potassium peroxydisulfates (label 1#, 2#, 3# and 4#) of the present embodiment are used for after recrystallization removal total nitrogen and ammonia nitrogen
The measure of water sample total nitrogen：
Take certain lake water water sample in Chinese workers campus.Based on standard method HJ636-2012, respectively with import potassium peroxydisulfate product,
And recrystallization four kinds of domestic potassium peroxydisulfate products (label 1#, 2#, 3# and 4#) of 1 time, 2 times and 3 times are measured to water sample.
The result of measure is as shown in table 1.
The performance of potassium peroxydisulfate product under the different recrystallization times conditions of table 1
Table large deviations refer to measured value and account for standard test value using the difference of import potassium peroxydisulfate product institute measurement result
Percentage.
Total nitrogen content by after 1 recrystallization, being determined can be seen that by the result of table 1 and import potassium peroxydisulfate is used
The result that product is determined is consistent, and reproducibility is good.I.e. domestic potassium peroxydisulfate product enters by the inventive method to total nitrogen
The measure requirement to environmental sample can be met after row effectively removal.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (2)
1. it is a kind of remove potassium peroxydisulfate in micro total nitrogen and ammonia nitrogen method, it is characterised in that comprise the following steps：
Pure water is heated to 50 DEG C of insulations, potassium peroxydisulfate stirring and dissolving to saturation state is subsequently adding, by gained saturation persulfuric acid
Crystallized as at a temperature of 4 DEG C after potassium solution sealing, taken out when crystal is no longer separated out, abandoning supernatant cleans crystalline substance with 4 DEG C of pure water
Body, then dries at a temperature of 50 DEG C, obtains removing the potassium peroxydisulfate after micro total nitrogen and ammonia nitrogen.
2. it is according to claim 1 it is a kind of remove potassium peroxydisulfate in micro total nitrogen and ammonia nitrogen method, it is characterised in that：Institute
State cleaned with 4 DEG C of pure water crystal number of times be 3 times.
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| CN201710152018.7A CN106865503A (en) | 2017-03-15 | 2017-03-15 | A kind of method of micro total nitrogen and ammonia nitrogen in removal potassium peroxydisulfate |
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| CN201710152018.7A CN106865503A (en) | 2017-03-15 | 2017-03-15 | A kind of method of micro total nitrogen and ammonia nitrogen in removal potassium peroxydisulfate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116119623A (en) * | 2023-01-29 | 2023-05-16 | 西陇科学股份有限公司 | Production method of environment-friendly high-purity potassium persulfate |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201746323U (en) * | 2010-05-24 | 2011-02-16 | 上海海洋大学 | Apparatus for purifying potassium peroxydisulfate in lab |
| CN104176748A (en) * | 2014-08-15 | 2014-12-03 | 广州衡创测试技术服务有限公司 | Method for purifying potassium persulfate |
| CN104568804A (en) * | 2015-01-30 | 2015-04-29 | 四川清和科技有限公司 | Method for detecting total nitrogen and total phosphorus of drainage basin |
| CN104596969A (en) * | 2015-01-30 | 2015-05-06 | 四川清和科技有限公司 | Rapid analysis method for total nitrogen in watershed |
| CN105016306A (en) * | 2014-04-23 | 2015-11-04 | 天津市光复科技发展有限公司 | Preparation method of high-purity low-nitrogen potassium persulfate |
| CN105565278A (en) * | 2014-10-14 | 2016-05-11 | 天津市光复科技发展有限公司 | Preparation method of high-purity low-nitrogen potassium persulfate |
-
2017
- 2017-03-15 CN CN201710152018.7A patent/CN106865503A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201746323U (en) * | 2010-05-24 | 2011-02-16 | 上海海洋大学 | Apparatus for purifying potassium peroxydisulfate in lab |
| CN105016306A (en) * | 2014-04-23 | 2015-11-04 | 天津市光复科技发展有限公司 | Preparation method of high-purity low-nitrogen potassium persulfate |
| CN104176748A (en) * | 2014-08-15 | 2014-12-03 | 广州衡创测试技术服务有限公司 | Method for purifying potassium persulfate |
| CN105565278A (en) * | 2014-10-14 | 2016-05-11 | 天津市光复科技发展有限公司 | Preparation method of high-purity low-nitrogen potassium persulfate |
| CN104568804A (en) * | 2015-01-30 | 2015-04-29 | 四川清和科技有限公司 | Method for detecting total nitrogen and total phosphorus of drainage basin |
| CN104596969A (en) * | 2015-01-30 | 2015-05-06 | 四川清和科技有限公司 | Rapid analysis method for total nitrogen in watershed |
Non-Patent Citations (3)
| Title |
|---|
| 杨森泉: "提纯过硫酸钾以满足总氮测定要求", 《广东化工》 * |
| 邓君杰 等: "重结晶-缓慢冷却法在提纯过硫酸钾的应用", 《资源节约与环保》 * |
| 隋伟 等: "重结晶法提纯过硫酸钾降低空白值的探讨", 《治淮》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116119623A (en) * | 2023-01-29 | 2023-05-16 | 西陇科学股份有限公司 | Production method of environment-friendly high-purity potassium persulfate |
| CN116119623B (en) * | 2023-01-29 | 2023-08-15 | 西陇科学股份有限公司 | Production method of environment-friendly high-purity potassium persulfate |
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Application publication date: 20170620 |