CN109541128A - The measuring method of manganese content in alkali formula manganese chloride - Google Patents
The measuring method of manganese content in alkali formula manganese chloride Download PDFInfo
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Abstract
The invention discloses a kind of measuring methods of manganese content in alkali formula manganese chloride comprising the steps of: (1) claims sample: alkali formula manganese chloride sample being claimed to be placed in container；(2) hydrochloric acid solution, PAN indicator, EDTA-2Na standard solution and EDTA-Cu solution preparation of reagents: are prepared；(3) pre-treatment: prepared hydrochloric acid solution is added in container, and water is added after heating for dissolving, then adjusts solution ph and prepared EDTA-Cu solution and PAN indicator is added；(4) it titrates；(5) the content X of manganese in alkali formula manganese chloride sample is calculated.The measuring method that the present invention is used to measure manganese content in alkali formula manganese chloride has many advantages, such as that easy to operate, measurement accuracy is high, reproducible, monitoring for manganese content in alkali formula manganese chloride and all has significance to the popularization as early as possible of alkali formula chlorination manganese product.
Description
Technical field
The present invention relates to quantitative analysis method field more particularly to a kind of measuring methods of manganese content.
Background technique
Manganese is arginase, enzyme proline, RNA polymerase, Mn-SOD (Mn-SOD), carboxylase
The constituent of enzyme etc., and the activity factor of many enzymes such as phosphorylase, aldolase, transferase, hydrolase in vivo.It is dynamic
Object manganese deficiency may occur in which that feed intake decline, decreased growth, efficiency of feed utilization reduces, bone is abnormal, incoordination and breeding function are abnormal
Phenomena such as.
Application of the alkali formula manganese chloride as feed addictive in livestock and poultry, external also someone carried out research such as:
A.K.Conly and R.Poureslami.Tolerance and efficacy oftribasic manganese
Chloride in growing broiler chickens.2012Poultry Science 91:1633-1640 (grind by test
Alkali formula manganese chloride is studied carefully to the tolerance and validity of growth broiler chicken).
X-XRD figure of the foreign countries in measuring alkali formula manganese chloride when manganese content mainly using powder compares estimation with reference substance
Product purity and manganese content.In order to promote alkali formula chlorination manganese product as early as possible at home, simple and convenient, widely used alkali formula is needed
The detection method of manganese chloride.Wherein, the content of manganese in the titration Accurate Determining alkali formula manganese chloride for how using covering surface most wide
It is mostly important.
Standard GB/T/T1506-2002 " the measurement potentiometric titration and ferrous ammonium sulfate titration of manganese ore manganese content "
In ferrous ammonium sulfate titration manganese content have the disadvantage that (1) sample pre-treatments are too complicated；(2) it needs 220
Ammonium nitrate is added at DEG C -240 DEG C makes bivalent manganese complete oxidation.But water boiling point is 100 DEG C, if being heated to 220 DEG C -240 DEG C,
Ie in solution is difficult to hold bivalent manganese just complete oxidation close to being evaporated.Temperature is too low, when ammonium nitrate oxidation is added, Mn2+It is oxidized to
Mn3+Not exclusively, cause measurement result relatively low；Temperature is excessively high, generates sticky pyrophosphate, it is inclined to also result in measurement result
It is low.(3) titration temperature requires stringent, it is necessary to assure at 60 DEG C, Tai Gao or the too low progress for being unfavorable for complexation reaction make terminal
Variation is fuzzy, it is difficult to judge.(4) the addition time of indicator is not easy to grasp, and this method requires to add when about 1mL before terminal
Enter chromium black T indicator, since terminal itself is difficult to determine, operation is not only difficult but also influences measurement result accuracy.
Mention in green " research of the manganese sulfate measuring method " text of official: there are also EDTA titrations for the measurement of manganese, including
The direct compleximetry of EDTA and Complexometric B ack-Titration method.Both use eriochrome black T as indicator, pH value is complexed in eriochrome black T optimum
It is 9~10.5.But divalent manganesetion precipitating initial pH value be 8.1, so divalent manganesetion pH be 9~10.5 when
Start to precipitate, the solution to be titrated that pH value is 9~10.5 has become cloudy, and generates manganous hydroxide, and manganous hydroxide is molten in alkalinity
It is unstable in liquid, disproportionated reaction occurs immediately: 2Mn (OH)3=Mn (OH)2+MnO2+2H2O influences the accuracy of result.
It is mentioned in Zhong Guoqing " feed grade manganese sulfate study on determination method " text: after feed grade manganese sulfate is dissolved with water,
The buffer solution and EDTA-Cu solution of pH=5.4 is added, is given instruction agent with PAN, titrates manganese with EDTA.But alkali formula manganese chloride
It is not soluble in water, it cannot directly apply manganese content in measuring method measurement alkali formula manganese chloride above.Alkali formula manganese chloride directly adds
The buffer solution for entering pH=5.4 is also difficult to dissolve, and pH value is 5.4 close to neutrality, and divalent manganesetion is easy under heating state
Hydrolysis further becomes insoluble matter manganese oxide after generating manganous hydroxide, and manganese oxide continues oxidation and becomes manganese dioxide.
Therefore, the measuring method of manganese content in the alkali formula manganese chloride that one kind is easy to operate, measurement accuracy is high is researched and developed
It is of great significance to the popularization as early as possible of alkali formula chlorination manganese product.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, one kind is provided
The measuring method of manganese content in alkali formula manganese chloride easy to operate, measurement accuracy is high, reproducible.It is asked to solve above-mentioned technology
Topic, technical solution proposed by the present invention are as follows:
The measuring method of manganese content in a kind of alkali formula manganese chloride comprising the steps of:
(1) claim sample: alkali formula manganese chloride sample being claimed to be placed in container；
(2) hydrochloric acid solution, PAN indicator (PAN is 1- (2- pyridylazo)-beta naphthal), EDTA- preparation of reagents: are prepared
2Na standard solution and EDTA-Cu solution；
(3) pre-treatment: prepared hydrochloric acid solution is added in container, water is added after heating for dissolving, then adjust pH value of solution
It is worth and prepared EDTA-Cu solution and PAN indicator is added；
(4) it titrates: with the solution obtained after pre-treatment in prepared EDTA-2Na standard solution titration step (3), directly
Becoming green from aubergine to solution is terminal, measures the volume v of used EDTA-2Na standard solution；
(5) the content X of manganese in alkali formula manganese chloride sample can be obtained using following formula, formula is as follows:
Wherein, X --- the content of manganese in alkali formula manganese chloride；
C --- EDTA-2Na concentration of standard solution, unit mol/L；
V --- the volume of the EDTA-2Na standard solution of titration consumption, Unit/mL；
The molal weight of M --- manganese；
M --- the weight of alkali formula manganese chloride sample, unit g.
In said determination method, it is preferred that claim in sample step, the quality m of weighed alkali formula manganese chloride sample is
0.0800g-0.1200g, when weighing, are accurate to 0.0001g.
In said determination method, it is preferred that impurity elements of ferrum in alkali formula manganese chloride sample, copper, zinc, lead content be ppm
Rank.The above-mentioned impurity element contained does not influence measurement result substantially, in addition, very low based on above-mentioned iron content, the present invention exists
It is not necessary that ammonium fluoride masking iron is added in titration process.
In said determination method, it is preferred that in preparation of reagents step, hydrochloric acid solution includes 1+1 hydrochloric acid, 1+5 hydrochloric acid；
The specific preparation of 1+1 hydrochloric acid includes: that 1 volume of water is added in 1 volume concentrated hydrochloric acid to shake up, and is made into 1+1 hydrochloric acid；
The specific preparation of 1+5 hydrochloric acid includes: that 5 volume of water are added in 1 volume concentrated hydrochloric acid to shake up, and is made into 1+5 hydrochloric acid；
The specific preparation of PAN indicator includes: that 1g PAN is added to dissolution in the ethanol solution of 200mL to shake up, and is made into
5g/L PAN ethanol solution；
The specific preparation of EDTA-2Na standard solution includes: according to national standard " GB/T 601-2016 chemical reagent standard
The preparation of titration solution " in " 4.15 disodium ethylene diamine tetraacetate standard titration solution " compound concentration c be 0.0480-
The EDTA-2Na standard solution of 0.0520mol/L；
The specific preparation of EDTA-Cu solution includes: the CuSO for taking 0.05mol/L4Solution 20mL is adjusted molten with 1+5 hydrochloric acid
Liquid pH value is acidity, 2 drop PAN indicator is added, with the titration of EDTA-2Na standard solution until solution becomes green from red, i.e.,
Obtain EDTA-Cu solution.
In said determination method, it is preferred that the concrete operations of pre-treatment include: after 10-20mL1+1 hydrochloric acid is added, logical
2-10min is placed in wind kitchen until the solution in container becomes brownish black clear solution, and then small fire heating container is until solution
It becomes colorless to flaxen clear solution, is moved away from heat source, rinse bottle wall with water (a small amount of water), it is cooling, add 100mL water to shake
It is even, then solution ph is adjusted with lye, and EDTA-Cu solution and PAN indicator is added, complete pre-treatment.Said determination method
In, using 1+1 dissolving with hydrochloric acid alkali formula manganese chloride sample.Reason is as follows: 1. solubility of the alkali formula manganese chloride sample in diluted acid compared with
Difference, the solubility in high concentrated acid are preferable.2. solvability of the alkali formula manganese chloride sample in hydrochloric acid, sulfuric acid, phosphoric acid, with salt
The solvability of acid is best.Manganese nitrate can be generated by not using nitric acid dissolution to allow for after alkali formula manganese chloride dissolves in nitric acid,
Manganese nitrate heating is precipitated manganese dioxide and releases nitrogen oxide gas.It does not use mixture of sulfuric phosphoric acid to allow for product and can generate not dissolving in
The manganese phosphate of water.3. the reason of not using concentrated hydrochloric acid to dissolve alkali formula manganese chloride sample is volatile for concentrated hydrochloric acid, heating state is brighter
It is aobvious.Dissolution alkali formula manganese chloride sample can satisfy using 1+1 hydrochloric acid, while bivalent manganese being prevented to be oxidized to the manganese ion of high-valence state.
Meanwhile the volume of the volume ratio concentrated hydrochloric acid of 1+1 hydrochloric acid is big, heating when, is not easy to be evaporated.4. because when concentration of hydrochloric acid is higher, meeting
Divalent manganesetion can be prevented by oxygen in entire preceding processing and titration process at divalent manganesetion value Mn ion reduction
Change, does not need additionally to add antioxidant such as hexamethylenetetramine etc..In above-mentioned pre-treatment operation, 10-20mL 1+1 salt is added
Needing to place 2-10min after acid is because the acidity of 1+1 hydrochloric acid dissolves the speed of alkali formula manganese chloride relatively without concentrated hydrochloric acid height
Slowly, after placing 2-10min, macroscopic alkali formula manganese chloride particle has disappeared, and product has been dissolved into small molecule state, this
When reheat and become colorless to flaxen clear solution, product dissolution is complete.But it is if straight without placing after acid adding
Heating is connect, a small amount of brownish black particulate matter can be remained after the completion of heating, in solution, influences testing result.
In said determination method, it is preferred that small fire heats solution temperature in container time control container and is no more than 100 DEG C.
In said determination method, it is preferred that in pre-treatment step, add 100mL water to shake up and adjust solution ph with lye
Between be additionally added 1mL 1+1 sulfuric acid, the specific preparation of 1+1 sulfuric acid are as follows: the 1 volume concentrated sulfuric acid is added in 1 volume of water and is shaken up, is matched
At 1+1 sulfuric acid.The purpose that sulfuric acid is added is not configured to better sample dissolution, but for the Pb in precipitation solution2+、Ca2+Deng
Impurity.Also, impurity content is seldom, and precipitating does not need to filter, and does not influence to titrate, but can reduce titration results and true value it
Between deviation.
In said determination method, it is preferred that lye is the sodium hydroxide solution that mass concentration is 10-20%.Sodium hydroxide
Cheap, free from extraneous odour is cheap unlike the irritant smell of ammonium hydroxide, and it is fast to adjust pH value speed.Concentration of sodium hydroxide solution
It is excessively high, it adjusts pH value and be easy to cause excessively high generation manganous hydroxide (II) precipitating of part alkalinity；Concentration is too low, adjusts pH value used time mistake
It is long, and cause the volume of entire solution system excessive, it is unfavorable for subsequent titration operation.
In said determination method, it is preferred that in pre-treatment step, adjusting solution ph is 2-4, and it is molten to control EDTA-Cu
The pH value of liquid is 2-4.The color change interval of PAN indicator is 2-12, but adjusts pH value using lye in actual operation, is not being had
In the case where having buffer solution, pH > 4.5 is easy that manganous hydroxide (II) precipitating is precipitated, forms suspension.The pH of pretreatment solution
Value is consistent with EDTA-Cu solution pH value, is to prevent error to make to titrate environment unification.And divalent manganesetion is in closely
Property into alkaline environment, in hot water environment may hydrolysis generate manganous hydroxide, be then oxidized to high price manganese ion.And in acidity
Under the conditions of, divalent manganesetion hydrolysis ability substantially reduces, and a possibility that being oxidized to high price manganese ion is much smaller.
In said determination method, it is preferred that in pre-treatment step, adjusting solution ph is 3-4, and it is molten to control EDTA-Cu
The pH value of liquid is 3-4.Show that the small effect of pH value acidity is more preferable by the theoretical research to contamination precipitation, choosing pH value is 3-4
It is more appropriate.
Ammonium fluoride masking iron is added without in said determination method, first is that because the environment of ammonium fluoride masking iron is alkalinity
Environment has little influence on measurement result second is that the iron contained in sample is ppm rank.
Compared with the prior art, the advantages of the present invention are as follows:
The present invention is used to measure the measuring method of manganese content in alkali formula manganese chloride with easy to operate, measurement accuracy is high, again
The advantages that renaturation is good, monitoring for manganese content in alkali formula manganese chloride and all has the popularization as early as possible of alkali formula chlorination manganese product
Significance.
Specific embodiment
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
The reagent that following embodiment uses is that analysis is pure, and water is deionized water.
The flat shape measurement of embodiment 1:()
The measuring method of manganese content in a kind of alkali formula manganese chloride comprising the steps of:
(1) sample: weighing m is referred to as 0.1023g, 0.1012g alkali formula manganese chloride sample (flat shape sample), is respectively placed in triangular flask
In；
(2) main agents are prepared:
1+1 hydrochloric acid: 1 volume of water is added in 1 volume concentrated hydrochloric acid and is shaken up, 1+1 hydrochloric acid is made into；
1+5 hydrochloric acid: 5 volume of water are added in 1 volume concentrated hydrochloric acid and are shaken up, 1+5 hydrochloric acid is made into；
1+1 sulfuric acid: the 1 volume concentrated sulfuric acid is added in 1 volume of water and is shaken up, 1+1 sulfuric acid is made into；
PAN indicator: 1gPAN is added to dissolution in the ethanol solution of 200ml and is shaken up, 5g/LPAN ethanol solution is made into；
EDTA-2Na standard solution: according to the national standard " system of GB/T 601-2016 chemical reagent standard titration solution
It is standby " in " 4.15 disodium ethylene diamine tetraacetate standard titration solution " compound concentration c be 0.05178mol/L EDTA-2Na standard
Solution；
EDTA-Cu solution: the CuSO of 0.05mol/L is taken4Solution 20mL is 3 with 1+5 salt acid for adjusting pH value, and 2 drops are added
The EDTA-2Na standard solution that PAN indicator is 0.05178mol/L with concentration be titrated to red and become green until to get arriving
EDTA-Cu solution；
(3) preparation of pretreatment solution: solution becomes brownish black suspension after 15mL 1+1 hydrochloric acid is added in triangular flask,
Place 5min in ventilating kitchen until solution is brownish black clear solution, small fire heating (be lower than 100 DEG C) to solution it is slightly boiled after become
For flaxen clear solution, it is moved away from heat source, bottle wall is rinsed with a small amount of water and adds 100mL water to shake up after being cooled to about 70 DEG C, then
Adjusting pH value with 20% caustic lye of soda is 3, and 5mL EDTA-Cu solution and 2 drop PAN indicator is added；
(4) it titrates: being titrated with the EDTA-2Na standard solution of 0.05178mol/L, until solution is by aubergine in triangular flask
Becoming green is terminal, and it is 19.57mL, 19.43mL that consumption EDTA-2Na standard solution v respectively, which is calculated, according to following
Formula calculating learns that the manganese content X of alkali formula manganese chloride is respectively 54.42%, 54.62%, and relative deviation RSD is 0.26%, variance
It is 2.00 × 10-6。
Embodiment 2 (personnel's comparison):
Another difference personnel repeat a kind of measuring method of manganese content in alkali formula manganese chloride comprising the steps of:
(1) sample: weighing m is referred to as 0.1107g, 0.1096g alkali formula manganese chloride sample (with 1 sample of embodiment, for flat shape sample),
It is respectively placed in triangular flask；
(2) main agents are prepared:
Reagent 1+1 hydrochloric acid, 1+5 hydrochloric acid and the 1+1 sulfuric acid prepared using embodiment 1；
EDTA-Cu solution: the CuSO of 0.05mol/L is taken4Solution 20mL is 2 with 1+5 salt acid for adjusting pH value, and 2 drops are added
The EDTA-2Na standard solution that PAN indicator is 0.05178mol/L with concentration be titrated to red and become green until to get arriving
EDTA-Cu solution；
(3) preparation of pretreatment solution: solution becomes brownish black suspension after 20mL 1+1 hydrochloric acid is added in triangular flask,
Place 10min in ventilating kitchen until solution is brownish black clear solution, small fire heating (be lower than 100 DEG C) to solution it is slightly boiled after become
For flaxen clear solution, it is moved away from heat source, bottle wall is rinsed with a small amount of water and adds 100mL water to shake up after being cooled to about 70 DEG C, then
Adjusting pH value with 12% caustic lye of soda is 2, and 5mL EDTA-Cu solution and 2 drop PAN indicator is added；
(4) it titrates: being titrated with the EDTA-2Na standard solution of 0.05178mol/L, until solution is by aubergine in triangular flask
Becoming green is terminal, and it is 21.25mL, 21.00mL that consumption EDTA-2Na standard solution v respectively, which is calculated, according to following
Formula calculating learns that the manganese content X of alkali formula manganese chloride is respectively 54.61%, 54.51%, and relative deviation RSD is 0.34%, variance
It is 3.38 × 10-6。
Embodiment 3 (keeps sample and surveys again):
Sampling is resurveyed after keeping sample one month.
The measuring method of manganese content in a kind of alkali formula manganese chloride comprising the steps of:
(1) sample: weighing m is referred to as 0.1045g, 0.1038g alkali formula manganese chloride sample (with 1 sample of embodiment, for flat shape sample),
It is respectively placed in triangular flask；
(2) main agents are prepared:
Main agents are prepared:
1+1 hydrochloric acid: 1 volume of water is added in 1 volume concentrated hydrochloric acid and is shaken up, 1+1 hydrochloric acid is made into；
1+5 hydrochloric acid: 5 volume of water are added in 1 volume concentrated hydrochloric acid and are shaken up, 1+5 hydrochloric acid is made into；
1+1 sulfuric acid: the 1 volume concentrated sulfuric acid is added in 1 volume of water and is shaken up, 1+1 sulfuric acid is made into；
PAN indicator: 1gPAN is added to dissolution in the ethanol solution of 200ml and is shaken up, 5g/LPAN ethanol solution is made into；
EDTA-2Na standard solution: according to the national standard " system of GB/T 601-2016 chemical reagent standard titration solution
It is standby " in " 4.15 disodium ethylene diamine tetraacetate standard titration solution " compound concentration c be 0.05178mol/L EDTA-2Na standard
Solution；
EDTA-Cu solution: the CuSO of 0.05mol/L is taken4Solution 20mL is 4 with 1+5 salt acid for adjusting pH value, and 2 drops are added
The EDTA-2Na standard solution that PAN indicator is 0.05178mol/L with concentration be titrated to red and become green until to get arriving
EDTA-Cu solution；
(3) preparation of pretreatment solution: solution becomes brownish black suspension after 20mL 1+1 hydrochloric acid is added in triangular flask,
Place 10min in ventilating kitchen until solution is brownish black clear solution, small fire heating (be lower than 100 DEG C) to solution it is slightly boiled after become
For flaxen clear solution, it is moved away from heat source, bottle wall is rinsed with a small amount of water and adds 100mL water to shake up after being cooled to about 50 DEG C, then
Adjusting pH value with 10% caustic lye of soda is 4, and 5mL EDTA-Cu solution and 2 drop PAN indicator is added.
(4) it titrates: being titrated with the EDTA-2Na standard solution of 0.05042mol/L, until solution is by aubergine in triangular flask
Becoming green is terminal, and it is 20.54mL, 20.50mL that consumption EDTA-2Na standard solution v respectively, which is calculated, according to following
Formula calculating learns that the manganese content X of alkali formula manganese chloride is respectively 54.45%, 54.70%, and relative deviation RSD is 0.13%, variance
It is 5.00 × 10-6。
By the measurement of different personnel and different time, experimental result in integrated embodiment 1-3, as shown in table 1 below.
Table 1: the experimental result in embodiment 1-3 summarizes
It can be seen that from the detection data of upper table using manganese content in the method detection alkali formula manganese chloride in the present embodiment
Reproducibility and repeatability are preferable, and stability and accuracy are higher.
Claims (10)
1. the measuring method of manganese content in a kind of alkali formula manganese chloride, which is characterized in that comprise the steps of:
(1) claim sample: alkali formula manganese chloride sample being claimed to be placed in container；
(2) hydrochloric acid solution, PAN indicator, EDTA-2Na standard solution and EDTA-Cu solution preparation of reagents: are prepared；
(3) pre-treatment: prepared hydrochloric acid solution is added in container, water is added after heating for dissolving, then adjust solution ph simultaneously
Prepared EDTA-Cu solution and PAN indicator is added；
(4) it titrates: the solution obtained after pre-treatment in prepared EDTA-2Na standard solution titration step (3) is used, up to molten
It is terminal that liquid, which becomes green from aubergine, measures the volume v of used EDTA-2Na standard solution；
(5) the content X of manganese in alkali formula manganese chloride sample can be obtained using following formula, formula is as follows:
Wherein, X --- the content of manganese in alkali formula manganese chloride；
C --- EDTA-2Na concentration of standard solution, unit mol/L；
V --- the volume of the EDTA-2Na standard solution of titration consumption, Unit/mL；
The molal weight of M --- manganese
M --- the weight of alkali formula manganese chloride sample, unit g.
2. measuring method according to claim 1, which is characterized in that in the title sample step, weighed alkali formula manganese chloride
The quality m of sample is 0.0800g-0.1200g, and when weighing is accurate to 0.0001g.
3. measuring method according to claim 1, which is characterized in that impurity elements of ferrum in the alkali formula manganese chloride sample,
Copper, zinc, lead content be ppm rank.
4. measuring method according to any one of claim 1-3, which is characterized in that in the preparation of reagents step, institute
Stating hydrochloric acid solution includes 1+1 hydrochloric acid, 1+5 hydrochloric acid；
The specific preparation of the 1+1 hydrochloric acid includes: that 1 volume of water is added in 1 volume concentrated hydrochloric acid to shake up, and is made into 1+1 hydrochloric acid；
The specific preparation of the 1+5 hydrochloric acid includes: that 5 volume of water are added in 1 volume concentrated hydrochloric acid to shake up, and is made into 1+5 hydrochloric acid；
The specific preparation of the PAN indicator includes: to dissolve to shake up in the ethanol solution for be added to 1gPAN 200mL, is made into
5g/LPAN ethanol solution；
The specific preparation of the EDTA-2Na standard solution includes: according to national standard " GB/T601-2016 chemical reagent standard
The preparation of titration solution " in " 4.15 disodium ethylene diamine tetraacetate standard titration solution " compound concentration c be 0.0480-
The EDTA-2Na standard solution of 0.0520mol/L；
The specific preparation of the EDTA-Cu solution includes: the CuSO for taking 0.05mol/L4Solution 20mL is adjusted with the 1+5 hydrochloric acid
Solution ph is acidity, and the 2 drop PAN indicator are added, with EDTA-2Na standard solution titration until solution is by red
Become green to get EDTA-Cu solution is arrived.
5. measuring method according to claim 4, which is characterized in that the concrete operations of the pre-treatment include: that 10- is added
After 1+1 hydrochloric acid described in 20mL, 2-10min is placed until the solution in container becomes brownish black clear solution, so in ventilating kitchen
Small fire heating container is moved away from heat source until solution becomes colorless to flaxen clear solution afterwards, cooling, and 100mL water is added to shake up,
Solution ph is adjusted with lye again, and EDTA-Cu solution and PAN indicator is added, completes pre-treatment.
6. measuring method according to claim 5, which is characterized in that small fire heats solution temperature in container time control container
No more than 100 DEG C.
7. measuring method according to claim 5, which is characterized in that in the pre-treatment step, add 100mL water shake up with
It is adjusted with lye and is additionally added 1mL1+1 sulfuric acid, the specific preparation of 1+1 sulfuric acid between solution ph are as follows: the 1 volume concentrated sulfuric acid is added
It is shaken up into 1 volume of water, is made into 1+1 sulfuric acid.
8. measuring method according to claim 5, which is characterized in that the lye is the hydrogen that mass concentration is 10-20%
Sodium hydroxide solution.
9. measuring method according to any one of claim 1-3, which is characterized in that in the pre-treatment step, adjust
Solution ph is 2-4, and the pH value for controlling the EDTA-Cu solution is 2-4.
10. measuring method according to claim 9, which is characterized in that in the pre-treatment step, adjusting solution ph is
3-4, and the pH value for controlling the EDTA-Cu solution is 3-4.
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| CN113016705A (en) * | 2021-03-15 | 2021-06-25 | 上海海洋大学 | Control method of biological heat source in container culture tail water |
| CN114018911A (en) * | 2021-11-08 | 2022-02-08 | 河海大学 | Test bar for rapidly detecting content of manganese ions in water and preparation method and application thereof |
| CN114923750A (en) * | 2022-05-17 | 2022-08-19 | 安徽大学 | Method for quantitatively detecting manganous chloride |
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| CN114923750A (en) * | 2022-05-17 | 2022-08-19 | 安徽大学 | Method for quantitatively detecting manganous chloride |
| CN114923750B (en) * | 2022-05-17 | 2024-04-02 | 安徽大学 | Method for quantitatively detecting manganous chloride |
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