CN108645961A - A kind of method of content of iodine in measurement feedstuff - Google Patents
A kind of method of content of iodine in measurement feedstuff Download PDFInfo
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Abstract
The present invention relates to a kind of methods of content of iodine in measurement feedstuff, and this approach includes the following steps：1) it heats after mixing calcium iodate sample, sulfuric acid solution, water, is filtered, washed while hot later, collect filtrate and cleaning solution and mix, obtain prepare liquid；2) ferrous sulfate solution, starch indicator solution are added into prepare liquid respectively, being titrated to prepare liquid with sodium thiosulfate standard solution later becomes colorless, and content of iodine is calculated.Compared with prior art, the present invention can be used in the content of iodine in 1 10% calcium iodate of rapid and accurate determination feedstuff, and the buying and examination to feedstuff provide reference data, while having great importance safely to feed quality；Assay method agents useful for same source is wide, moderate, reproducible, the accurate and effective of measurement result.
Description
Technical field
The invention belongs to chemical composition detection technique field in feedstuff, it is related to content of iodine in a kind of measurement feedstuff
Method.
Background technology
Main constituents of the iodine as thyroid hormone, it is closely related with the basic metabolism of animal, it is that animal early stage is raw
Long necessary element.Common iodine complement agent domestic at present is mainly potassium iodide and calcium iodate, wherein potassium iodide is because of its chemistry
The drawbacks such as poor, the moisture-sensitive caking of stability, cause its applicability to be had a greatly reduced quality；Calcium iodate then have stability is good, be slightly soluble in water,
The almost non-hygroscopic, advantages such as bioavailability is high.Therefore, calcium iodate is widely used.For more accurately formula feed,
Measuring the purity of calcium iodate in feedstuff is just particularly important.
Currently, the chemical industry standard issued about detection calcium iodate purity《HG/T 2418-2011 feed grade acid iodide
Calcium》High-purity calcium iodate is only applicable to (in terms of iodine：61.8-62.8wt%), presently commercially available calcium iodate is all substantially
Mixed feed additive, purity is often relatively low, in terms of the mass percentage of iodine, common are 1% calcium iodate, 2% iodine
Sour calcium, 5% calcium iodate and 10% calcium iodate etc..If using chemical industry standard《2418-2011 feed grade calcium iodates of HG/T》
It can be even applicable in reluctantly to measure 10% calcium iodate, but for measuring lower 1% calcium iodate of purity, 2% calcium iodate and 5%
Calcium iodate is just less applicable in.The main reason is that：Since the content of iodine in 10% calcium iodate is higher, according to chemical industry standard
Method be measured, required for the volume of sodium thiosulfate that consumes be about 5-6 milliliters；And disappear required for 5% calcium iodate
The volume of the sodium thiosulfate of consumption only has 2-3 milliliters, and the volume of the sodium thiosulfate consumed required for 1% calcium iodate can be less,
Several milliliters of zero is only needed just to reach titration end-point when titration.Therefore, if measuring 1% acid iodide with the chemical industry standard method
Content of iodine in calcium, 2% calcium iodate and 5% calcium iodate, since the sodium thiosulfate volume consumed required for it is seldom, therefore significantly
Titration error is increased, the accuracy of measurement result is influenced.
Although country still has standard for measuring the content of iodine in feed, i.e.,《The survey of iodine in GB/T 13882-2010 feeds
Determine ferric rhodanate-nitrous acid Catalytic Kinetics》, but this method operation difficulty height, complex steps, need reagent preparation it is more, survey
Determine the content of iodine that result stability is poor, is unsuitable in measurement 1-10% calcium iodates.
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of measurement feedstuffs
The method of middle content of iodine.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method of content of iodine in measurement feedstuff, this approach includes the following steps：
1) it heats after mixing calcium iodate sample, sulfuric acid solution, water, is filtered, washed while hot later, collect filtrate and washing
Liquid simultaneously mixes, and obtains prepare liquid；
2) ferrous sulfate solution, starch indicator solution are added into prepare liquid respectively, use sodium thiosulfate standard molten later
Liquid is titrated to prepare liquid and becomes colorless, and content of iodine is calculated.
Further, in step 1), in the calcium iodate sample, the mass percentage of iodine is 1-10%.
Further, in step 1), in the sulfuric acid solution, H2SO4Mass percentage be 18-22%.
Further, in step 1), the volume ratio of the sulfuric acid solution and water is 1:0.9-1.1, it is molten per 20mL sulfuric acid
0.5-3g calcium iodate samples are added in liquid.Wherein, 1% calcium iodate weighs 3g or so, 2% calcium iodate weighs 2g or so, 5% acid iodide
Calcium weighs 1g or so, 10% calcium iodate weighs 0.5g or so.
Further, it in step 1), in the heating process, is removed after being heated to boiling.
Further, in step 2), in the ferrous sulfate solution, the mass-volume concentration of ferrous sulfate is 45-
55g/L。
Further, the volume ratio of the ferrous sulfate solution and sulfuric acid solution in step 1) is 2-4:20.
Further, in step 2), the mass-volume concentration of the starch indicator solution is 8-12g/L.
The present invention is in practical application, can increase blank test (being not added with calcium iodate sample, other identical), to improve inspection
Survey precision.
The present invention and chemical industry standard《HG/T 2418-2011 feed grade calcium iodates》It compares, there is following advantage：
(1) limitation of the chemical industry standard to calcium iodate purity testing range is overcome；
(2) perchloric acid has strong oxidizing property and corrosivity, contact with organic matter, heat easily sets off an explosion, and has centainly
Danger, the present invention replaces perchloric acid with 20% or so sulfuric acid solution, improves the safety of experimental implementation；
(3) when measuring the content of iodine in low-purity calcium iodate according to chemical industry standard, it is necessary to sample weighting amount must be increased, weighed
The calcium iodate sample of 3g, which takes around addition 50mL perchloric acid, just can be such that calcium iodate sample is completely dissolved under the conditions of low-grade fever, herein
In strongly acidic solution, it will so that sodium thiosulfate standard solution is decomposed, influence the accuracy of experimental result；
(4) the method for the present invention operating process is convenient, is out analyzed without pipetting part test solution after constant volume again；
(5) present invention replaces potassium iodide with ferrous sulfate, can avoid influence of the iodine in potassium iodide to testing result, more
Be conducive to the buying to feedstuff and examination, avoid the adulterated problem of feedstuff to a certain extent.
The present invention and national standard《Iodide determination ferric rhodanate-nitrous acid catalytic kinetic in GB/T 13882-2010 feeds
Method》It compares, there is following advantage：
(1) reagent preparation is less；
(2) operating process is easy, and experiment takes shorter；
(3) test result is stable, reproducible, error is small.
Compared with prior art, the invention has the characteristics that：
1) present invention can be used in the content of iodine in rapid and accurate determination feedstuff 1-10% calcium iodates, to feedstuff
Buying and check and accept reference data be provided, while having great importance safely to feed quality；
2) assay method agents useful for same of the present invention source is wide, moderate, reproducible, the accurate and effective of measurement result；
3) the present invention overcomes the limitations of calcium iodate detection range in the prior art, and it is relatively low right to avoid solution ph
The adverse effect of sodium thiosulfate standard solution stability can be realized within a short period of time in feedstuff 1-10% calcium iodates
The accurate detection of content of iodine.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.The present embodiment is based on the technical solution of the present invention
Implemented, give detailed embodiment and specific operating process, but protection scope of the present invention be not limited to it is following
Embodiment.
Embodiment 1：
Reagent needed for 1 test preparation
1.1 sulfuric acid solution：20%H2SO4Solution；
1.2 ferrous sulfate solution：50g/L FeSO4Solution；
1.3 sodium thiosulfate standard solution：c(Na2S2O3)≈0.1mol/L；
1.4 starch indicator solutions：10g/L.
The preparation of 2 samples
Calcium iodate sample 50g or so to be detected is taken, is put in closed container, it is labelled.
3 measure sample
It weighs calcium iodate sample 0.5-3g and (is accurate to 0.0002g, wherein 1% calcium iodate weighs 3g or so, 2% calcium iodate
Weigh 2g or so, 5% calcium iodate weighs 1g or so, 10% calcium iodate weighs 0.5g or so), it is placed in 250mL beakers, is added
20% sulfuric acid solutions of 20mL, 20mL water are placed in heating on electric furnace and boil dissolved samples, uses middling speed quantitative filter paper to filter while hot, use
30mL hot water washs filter residue several times, and filtrate and cleaning solution are collected in 250mL iodine flasks, and 3mL 50g/L ferrous sulfate is added
Solution, rapid water seal, shakes up, and 5min is stood in dark place.With sodium thiosulfate standard solution be titrated to solution in it is light yellow when, add
Enter 3mL 10g/L starch indicator solutions, it is terminal to continue to be titrated to blue and disappear.It is carried out at the same time blank test.
Blank test：In addition to being not added with calcium iodate sample, the type and amount and sample solution phase of other operations and addition reagent
Together.
4 results calculate
Acid iodide calcium content is calculated with the mass fraction X (%) of iodine (I) according to following equation：
In formula：
The exact value of c-Concentration of Sodium Thiohsulfate Standard Solution, unit are mole every liter (mol/L)；
The volumetric quantities of the sodium thiosulfate standard solution of V-titration consumption, unit are milliliter (mL)；
V0The volumetric quantities of the sodium thiosulfate standard solution of-blank test titration consumption, unit are milliliter (mL)；
1/5 (M=25.38) of M-iodine (I) molal weight, unit are gram every mole (g/mol).
The testing principle of this method is：
Ca(IO3)2With the reagent FeSO being added4Reaction generates I in acid condition2Simple substance and Fe2(SO4)3, solution exists
It is added after starch indicator solution in blue, with product (I2Simple substance and Fe2(SO4)3) reacted with the continuous of sodium thiosulfate, work as I2
After total overall reaction, blue disappears.
Reaction equation is：
Ca(IO3)2+10FeSO4+6H2SO4=CaSO4+I2+5Fe2(SO4)3+6H2O
2Na2S2O3+I2=Na2S4O6+2NaI
2S2O3 2-+4Fe3+→S4O6 2-+4Fe2+
Wherein, the sample weighting amount of calcium iodate sample is preferably controlled between 0.5-3.0g, wherein 1% calcium iodate is optimal for the left sides 3g
It is 2g or so that right, 2% calcium iodate is optimal, 5% calcium iodate it is optimal be 1g or so, optimal 10% calcium iodate is 0.5g or so.
Wherein, the addition of 20% sulfuric acid solution is 15-25mL, and optimal is 20mL.
Wherein, the addition of 50g/L ferrous sulfate solutions is 2-5mL, and optimal is 3mL.
Pass through the above-mentioned conclusion of following experimental verification.
1, the same a collection of 10% calcium iodate sample of 20% sulfuric acid solution of different volumes, measurement result such as following table is added：
| Serial number | 20% sulfuric acid solution volume, mL | Content of iodine, % |
| 1 | 5 | 9.66 |
| 2 | 10 | 9.82 |
| 3 | 15 | 9.99 |
| 4 | 20 | 10.00 |
| 5 | 25 | 10.03 |
| 6 | 30 | 9.96 |
According to upper table as can be seen that between the addition of 20% sulfuric acid solution is preferably controlled in 15-25mL, to ensure sulfuric acid
Amount of solution is enough, does not influence measurement result, ensures the stability of measurement result, and consider reagent cost, and optimal is 20mL.
2, the same a collection of 10% calcium iodate sample of different volumes 50g/L ferrous sulfate solutions is added, measurement result is as follows
Table：
| Serial number | 50g/L ferrous sulfate solution volumes, mL | Content of iodine, % |
| 1 | 1 | 9.58 |
| 2 | 2 | 9.99 |
| 3 | 3 | 10.00 |
| 4 | 5 | 10.01 |
| 5 | 7 | 10.02 |
| 6 | 9 | 10.02 |
According to upper table as a result, since there are little deviations for content of iodine in different calcium iodate samples, to ensure ferrous sulfate
Addition is enough, does not influence measurement result, and in view of factors such as reagent costs, therefore the addition of 50g/L ferrous sulfate is best
In 2-5mL, optimal is 3mL for control.
3, this method is reproducible, measures with a collection of 1% calcium iodate sample, repeated measurement result such as following table：
As can be seen from the above table, this method is reproducible.
Embodiment 2：
1) instrument and equipment
Assay balance (being accurate to 0.0001g mono-), electric furnace (2500W), 250mL beakers, 250mL iodine flasks, funnel, in
Fast quantitative filter paper, 25mL buret single tracks.
2) environmental requirement
Room temperature：20-25℃.
In the present embodiment, experimental group detection process is same as Example 1.
1% calcium iodate sample is taken to be divided into more parts, with improved chemical industry standard《HG/T 2418-2011 feed grade iodine
Sour calcium》For control group 1, with national standard《Iodide determination ferric rhodanate-nitrous acid catalysis is dynamic in GB/T 13882-2010 feeds
Mechanical Method》For control group 2 three kinds of methods are compared respectively, iodine in same a collection of 1% calcium iodate sample is contained using this method as experimental group
The measurement result of amount.Wherein, in 1 method of control group, in existing chemical industry standard《HG/T 2418-2011 feed grade acid iodide
Calcium》On the basis of, in order to measure low-purity calcium iodate sample, sodium thiosulfate standard solution is diluted.Content of iodine is tested
The results are shown in table below：
| 1% calcium iodate sample | Control group 1 | Control group 2 | Experimental group |
| 1 | 0.99% | 0.90% | 1.01% |
| 2 | 1.02% | 1.05% | 1.00% |
| 3 | 1.01% | 0.97% | 1.00% |
| 4 | 0.97% | 1.04% | 1.01% |
| 5 | 1.02% | 0.95% | 1.01% |
2% calcium iodate sample is taken to be divided into more parts, with improved chemical industry standard《HG/T 2418-2011 feed grade iodine
Sour calcium》For control group 1, with national standard《Iodide determination ferric rhodanate-nitrous acid catalysis is dynamic in GB/T 13882-2010 feeds
Mechanical Method》For control group 2 three kinds of methods are compared respectively, iodine in same a collection of 2% calcium iodate sample is contained using this method as experimental group
The measurement result of amount.Wherein, in 1 method of control group, in order to measure low-purity calcium iodate sample, to sodium thiosulfate standard solution
It is diluted.Test result is as follows for content of iodine shown in table：
| 2% calcium iodate sample | Control group 1 | Control group 2 | Experimental group |
| 1 | 1.98% | 1.94% | 2.00% |
| 2 | 1.98% | 1.96% | 2.01% |
| 3 | 2.02% | 2.04% | 2.00% |
| 4 | 1.99% | 2.08% | 2.00% |
| 5 | 2.03% | 2.06% | 2.01% |
5% calcium iodate sample is taken to be divided into more parts, with improved chemical industry standard《HG/T 2418-2011 feed grade iodine
Sour calcium》For control group 1, with national standard《Iodide determination ferric rhodanate-nitrous acid catalysis is dynamic in GB/T 13882-2010 feeds
Mechanical Method》For control group 2 three kinds of methods are compared respectively, iodine in same a collection of 5% calcium iodate sample is contained using this method as experimental group
The measurement result of amount.Wherein, in 1 method of control group, in order to measure low-purity calcium iodate sample, to sodium thiosulfate standard solution
It is diluted.Test result is as follows for content of iodine shown in table：
| 5% calcium iodate sample | Control group 1 | Control group 2 | Experimental group |
| 1 | 5.03% | 5.04% | 5.00% |
| 2 | 5.04% | 5.05% | 5.01% |
| 3 | 5.04% | 4.95% | 5.00% |
| 4 | 5.06% | 5.06% | 5.01% |
| 5 | 5.03% | 4.97% | 5.00% |
10% calcium iodate sample is taken to be divided into more parts, with improved chemical industry standard《HG/T 2418-2011 feed grades
Calcium iodate》For control group 1, with national standard《Iodide determination ferric rhodanate-nitrous acid catalysis in GB/T 13882-2010 feeds
KINETIC METHOD》Three kinds of methods are compared respectively in same a collection of 10% calcium iodate sample using this method as experimental group for control group 2
The measurement result of content of iodine.Test result is as follows for content of iodine shown in table：
| 5% calcium iodate sample | Control group 1 | Control group 2 | Experimental group |
| 1 | 9.93% | 9.90% | 10.00% |
| 2 | 10.04% | 9.94% | 10.00% |
| 3 | 9.98% | 10.05% | 10.01% |
| 4 | 10.05% | 10.06% | 10.01% |
| 5 | 9.98% | 9.96% | 10.00% |
Above-mentioned test result shows that the method for the present invention measures content of iodine in 1%-10% calcium iodates, with improved chemical industry
Professional standard《HG/T 2418-2011 feed grade calcium iodates》And national standard《Iodide determination in GB/T 13882-2010 feeds
Ferric rhodanate-nitrous acid Catalytic Kinetics》Compare, measurement result is more stable, more acurrate, therefore can be used this method pair 1%~
Content of iodine is measured in 10% calcium iodate.
Embodiment 3：
A kind of method of content of iodine in measurement feedstuff, this approach includes the following steps：
1) the calcium iodate sample by mass percentage for 1%, H2SO4Mass percentage be 22% sulfuric acid solution,
It heats after water mixing, is removed after being heated to boiling.It is filtered, washed, collects filtrate and cleaning solution and mixes while hot later, waited for
Survey liquid, wherein the volume ratio of sulfuric acid solution and water is 1:0.9,3g calcium iodate samples often are added in 20mL sulfuric acid solutions；
2) starch that ferrous sulfate solution that mass-volume concentration is 45g/L, mass-volume concentration are 12g/L is referred to respectively
Show that liquid is added into prepare liquid, being titrated to prepare liquid with sodium thiosulfate standard solution later becomes colorless, and iodine is calculated and contains
Amount, wherein the volume ratio of ferrous sulfate solution and sulfuric acid solution in step 1) is 1:10.
Embodiment 4：
A kind of method of content of iodine in measurement feedstuff, this approach includes the following steps：
1) the calcium iodate sample by mass percentage for 2%, H2SO4Mass percentage be 18% sulfuric acid solution,
It heats after water mixing, is removed after being heated to boiling.It is filtered, washed, collects filtrate and cleaning solution and mixes while hot later, waited for
Survey liquid, wherein the volume ratio of sulfuric acid solution and water is 1:1.1,2g calcium iodate samples often are added in 20mL sulfuric acid solutions；
2) starch that ferrous sulfate solution that mass-volume concentration is 55g/L, mass-volume concentration are 8g/L is referred to respectively
Show that liquid is added into prepare liquid, being titrated to prepare liquid with sodium thiosulfate standard solution later becomes colorless, and iodine is calculated and contains
Amount, wherein the volume ratio of ferrous sulfate solution and sulfuric acid solution in step 1) is 1:5.
Embodiment 5：
A kind of method of content of iodine in measurement feedstuff, this approach includes the following steps：
1) the calcium iodate sample by mass percentage for 5%, H2SO4Mass percentage be 20% sulfuric acid solution,
It heats after water mixing, is removed after being heated to boiling.It is filtered, washed, collects filtrate and cleaning solution and mixes while hot later, waited for
Survey liquid, wherein the volume ratio of sulfuric acid solution and water is 1:1,1g calcium iodate samples often are added in 20mL sulfuric acid solutions；
2) starch that ferrous sulfate solution that mass-volume concentration is 50g/L, mass-volume concentration are 10g/L is referred to respectively
Show that liquid is added into prepare liquid, being titrated to prepare liquid with sodium thiosulfate standard solution later becomes colorless, and iodine is calculated and contains
Amount, wherein the volume ratio of ferrous sulfate solution and sulfuric acid solution in step 1) is 3:20.
Embodiment 6：
A kind of method of content of iodine in measurement feedstuff, this approach includes the following steps：
1) the calcium iodate sample by mass percentage for 10%, H2SO4Mass percentage be 21% sulfuric acid it is molten
It heats after liquid, water mixing, is removed after being heated to boiling.It is filtered, washed, collects filtrate and cleaning solution and mixes while hot later, obtain
To prepare liquid, wherein the volume ratio of sulfuric acid solution and water is 1:1,0.5g calcium iodate samples often are added in 20mL sulfuric acid solutions；
2) starch that ferrous sulfate solution that mass-volume concentration is 52g/L, mass-volume concentration are 9g/L is referred to respectively
Show that liquid is added into prepare liquid, being titrated to prepare liquid with sodium thiosulfate standard solution later becomes colorless, and iodine is calculated and contains
Amount, wherein the volume ratio of ferrous sulfate solution and sulfuric acid solution in step 1) is 3:20.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be the present invention's
Within protection domain.
Claims (8)
1. a kind of method measuring content of iodine in feedstuff, which is characterized in that this approach includes the following steps：
1) it heats after mixing calcium iodate sample, sulfuric acid solution, water, is filtered, washed while hot later, collect filtrate and cleaning solution simultaneously
Mixing, obtains prepare liquid；
2) ferrous sulfate solution, starch indicator solution are added into prepare liquid respectively, are dripped later with sodium thiosulfate standard solution
It is fixed to become colorless to prepare liquid, content of iodine is calculated.
2. a kind of method measuring content of iodine in feedstuff according to claim 1, which is characterized in that in step 1),
In the calcium iodate sample, the mass percentage of iodine is 1-10%.
3. a kind of method measuring content of iodine in feedstuff according to claim 1, which is characterized in that in step 1),
In the sulfuric acid solution, H2SO4Mass percentage be 18-22%.
4. a kind of method measuring content of iodine in feedstuff according to claim 1, which is characterized in that in step 1),
The volume ratio of the sulfuric acid solution and water is 1:Often 0.5-3g calcium iodate samples are added in 20mL sulfuric acid solutions in 0.9-1.1.
5. a kind of method measuring content of iodine in feedstuff according to claim 1, which is characterized in that in step 1),
In the heating process, removed after being heated to boiling.
6. a kind of method measuring content of iodine in feedstuff according to claim 1, which is characterized in that in step 2),
In the ferrous sulfate solution, the mass-volume concentration of ferrous sulfate is 45-55g/L.
7. a kind of method measuring content of iodine in feedstuff according to claim 6, which is characterized in that the sulfuric acid
The volume ratio of ferrous iron solution and sulfuric acid solution in step 1) is 2-4:20.
8. a kind of method measuring content of iodine in feedstuff according to claim 1, which is characterized in that in step 2),
The mass-volume concentration of the starch indicator solution is 8-12g/L.
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