CN102001868A - Extraction method of available phosphorus and water soluble potassium in fertilizer - Google Patents
Extraction method of available phosphorus and water soluble potassium in fertilizer Download PDFInfo
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- CN102001868A CN102001868A CN2010101751067A CN201010175106A CN102001868A CN 102001868 A CN102001868 A CN 102001868A CN 2010101751067 A CN2010101751067 A CN 2010101751067A CN 201010175106 A CN201010175106 A CN 201010175106A CN 102001868 A CN102001868 A CN 102001868A
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Abstract
The invention relates to an extraction method of available phosphorus and water soluble potassium in fertilizer, in particular to a method for extracting available phosphorus and water soluble potassium in fertilizer by utilizing ultrasonic. The extraction method of the available phosphorus and water soluble potassium in the fertilizer of the invention comprises the following steps: preparing a sample to be tested; weighing the sample to be tested and placing the sample to be tested in a volumetric flask; adding extracting solution and mixing uniformly; and placing the volumetric flask in an ultrasonic device, and carrying out ultrasonic cavitation extraction. Compared with the prior art, the invention has the advantages that the available phosphorus and water soluble potassium in the fertilizer are extracted by utilizing the ultrasonic cavitation effect, thus the demands of rapid detection and cost reduction are met; and detection results are high in accuracy and conform to the international standard, and the extraction efficiency of the available phosphorus and water soluble potassium in the fertilizer are effectively enhanced.
Description
Technical field
The present invention relates to extraction of effective components in the fertilizer, relate in particular to the extracting method of available phosphorus in the fertilizer, water-soluble potassium.
Background technology
According to existing GB GB/8573-1999 standard, the extracting method of the available phosphorus in the fertilizer is: take by weighing the sample (claiming accurate to 0.0001g) that contains the about 100-200mg of available phosphorus with ten thousand/electronic balance, place the 250ml volumetric flask, adding 150ml is heated to 60 ℃ EDTA solution in advance, the jam-pack bottle stopper, shake volumetric flask sample is scattered in the solution, place 60 ℃ ± 1 ℃ water bath with thermostatic control vibrator, constant temperature vibration 1 hour.
According to existing GB GB/8574-2002 standard, the extracting method of the water-soluble potassium in the fertilizer is: take by weighing the sample (claiming accurate to 0.0001g) that contains the about 300-400mg of water-soluble potassium with ten thousand/electronic balance, place the 250ml triangular flask, add 150ml distilled water, shaking triangular flask is scattered in the solution sample, placed on the electric furnace heated and boiled 30 minutes, and quantitatively moved on in the 250ml volumetric flask after the cooling.
Available phosphorus by in the existing GB detection method extraction fertilizer of carrying out need vibrate 1 hour by constant temperature in water bath chader, could detect by constant volume after the cooling, and whole extraction time needs 90 minutes approximately; The extraction of water-soluble potassium needed heated and boiled 30 minutes, could detect by constant volume after the cooling, and whole extraction time needs 60 minutes approximately.
In sum, the method for available phosphorus, water-soluble potassium in the existing extraction fertilizer, the operating time is long, current consumption is high; Therefore be necessary to develop a kind of can solving the problems of the technologies described above, the available phosphorus in can rapid extraction fertilizer, the method for water-soluble potassium.
Summary of the invention
The method that the purpose of this invention is to provide available phosphorus, water-soluble potassium in a kind of rapid extraction fertilizer.
In order to solve the problems of the technologies described above, the contriver has carried out a large amount of experiments, discovery is in fertilizer nutrient mensuration process, utilize the ultrasonic cavitation effect, can make fierce at a high speed collision takes place between liquid particle, with the available phosphorus in the fertilizer sample, water-soluble potassium fast from sample separate dissolved in extracting solution, therefore available phosphorus, water-soluble potassium in can rapid extraction fertilizer, thus satisfy the rapid detection requirement.
According to above principle, the invention provides the extracting method of available phosphorus, water-soluble potassium in a kind of fertilizer, it comprises the following steps: to prepare testing sample; Take by weighing testing sample and be placed in the volumetric flask, add extracting solution and mix, place ultrasonic equipment to carry out ultrasonic cavitation in volumetric flask and extract.
The time that described ultrasonic cavitation extracts is 3 to 15 minutes; Described ultrasonic cavitation extracts employed ultrasonic frequency in 30KHz to 100KHz scope.
The Best Times that described ultrasonic cavitation extracts is 5 minutes; It is 60KHz that described ultrasonic cavitation extracts employed best ultrasonic frequency.
In the extraction of available phosphorus, described extracting solution is a kind of in salpeter solution, disodium EDTA (EDTA) solution or the neutral ammonium citrate solution.
The preparation composition of described salpeter solution is nitric acid and distilled water, and described salpeter solution concentration range is between (1+1) to (1+4); Described disodium EDTA (EDTA) strength of solution scope is between 30g/L to 60g/L; The preparation composition of described neutral ammonium citrate solution is citric acid and ammoniacal liquor.
The best compound concentration of described salpeter solution is (1+2); The best compound concentration of described EDTA solution is 37.5g/L.
In the extraction of water-soluble potassium, described extracting solution is a distilled water.
Described ultrasonic equipment is a groove type ultrasonic ripple cleanser, and described volumetric flask is to place the aqueous solution in the ultrasonic cleaner rinse bath to carry out the ultrasonic cavitation extraction.
Described testing sample is meant with the slot type reduction device through repeatedly taking out after the division, is crushed to all sample by the 0.5mm aperture sieve with pulverizer again.
It is described that what take by weighing that testing sample uses is ten thousand/electronic balance.
With respect to prior art, the extracting method of available phosphorus, water-soluble potassium has following advantage in the fertilizer of the present invention,
1, owing to adopt available phosphorus in the ultrasonic extraction fertilizer, make composition extraction time shorten to existing execution national standard method 1/18th, promptly 90 minute extraction time by national standard method shortens to 5 minutes, shortens the extraction time of available phosphorus in the fertilizer greatly;
2, owing to adopt water-soluble potassium in the ultrasonic extraction fertilizer, make composition extraction time shorten to existing execution national standard method 1/12nd, promptly 60 minute extraction time by national standard method shortens to 5 minutes, shortens the extraction time of water-soluble potassium in the fertilizer greatly;
3, the requirement that can not only satisfy rapid detection, reduces cost, and detected result accuracy height meet the GB requirement, effectively improved the extraction efficiency of available phosphorus and water-soluble potassium in the fertilizer.
Embodiment
In fertilizer nutrient mensuration process, utilize the ultrasonic cavitation effect to extract available phosphorus, water-soluble potassium in the fertilizer, it is the ultrasonic cavitation effect of utilizing ultrasonic equipment to produce, make fierce at a high speed collision takes place between liquid particle, with the available phosphorus in the fertilizer sample, water-soluble potassium fast from sample separate dissolved in extracting solution, so available phosphorus, water-soluble potassium in the energy rapid extraction fertilizer, thereby satisfy the rapid detection requirement, and save and detect cost.
The extracting method required equipment of available phosphorus, water-soluble potassium comprises ultrasonic equipment in the fertilizer of the present invention, wherein, the range of frequency that ultrasonic equipment is set is 30KHz to 100KHz, its optimum setting value is 60KHz, extraction time prolonged when frequency setting value was lower than optimum value, the too high noise that then causes of frequency setting value is excessive, pollutes Working environment.Ultrasonic equipment is a groove type ultrasonic ripple cleanser in the present embodiment.The extracting method of available phosphorus, water-soluble potassium in the fertilizer as detailed below.
Embodiment one
The extraction experimental implementation of available phosphorus is as follows in the fertilizer:
1. extracting solution preparation
Salpeter solution is the analytical pure nitric acid of 65%-68% and the distilled water compound concentration salpeter solution for (1+1) to (1+4) by concentration, and promptly the distilled water of the nitric acid of 1 part of volume and 2 parts of volumes mixes formulated.Wherein, (1+2) salpeter solution effect when extracting available phosphorus is best.And cross when low when salpeter solution concentration, can't extract the available phosphorus in the fertilizer fully.
2. preparation testing sample
With testing sample with the slot type reduction device through repeatedly taking out about 100g after the division, with pulverizer sample is crushed to all by the 0.5mm aperture sieve, mix, place cleaning, exsiccant weighing bottle.
3. available phosphorus in the ultrasonic extraction fertilizer
Take by weighing the fertilizer sample that contains the about 100-200mg of available phosphorus with ten thousand/electronic balance, weigh precisely to 0.0001g, place the 250ml volumetric flask, add the 150ml salpeter solution, shaking volumetric flask is scattered in the solution sample, volumetric flask is placed the aqueous solution in the ultrasonic cleaner rinse bath, open ultrasonic cleaner, carry out 3-15 minute ultrasonic extraction.Find that through experiment the best ultrasonic extraction time is 5 minutes.
By above-mentioned steps, same sample carries out parallel sample operation experiments under the same conditions.Now the test data with experimental record test data and GB extracting method compares, correlation data such as following table.
The test data of table 1 ultrasonic extraction available phosphorus and the test data contrast table of national standard method
From above-mentioned test-results, ultrasonic extraction extracts the replicate(determination) result of available phosphorus, and its absolute value of the bias is less than 0.12%, same sample revision test measurement result, and its absolute value of the bias meets requirement of experiment less than 0.09%; Compare with the former method of GB8573-1999, two kinds of method measurement result absolute differences meet the GB requirement less than 0.10%.But the national standard method that the time ratio of ultrasonic extraction available phosphorus is now carried out has shortened 18 times, and promptly 90 minute extraction time by national standard method shortens to 5 minutes.This shows the requirement that the method for the available phosphorus in the ultrasonic extraction fertilizer can not only satisfy rapid detection, reduce cost, and detected result accuracy height, meet the GB requirement, effectively improved the extraction efficiency of available phosphorus in the fertilizer.
Embodiment two
The extraction experimental implementation of water-soluble potassium is as follows in the fertilizer:
1. sampling
With sample to be extracted with the slot type reduction device through repeatedly taking out about 100g after the division, with pulverizer sample is crushed to all by the 0.5mm aperture sieve, mix, place cleaning, exsiccant weighing bottle.
2. the method for water-soluble potassium in the ultrasonic extraction fertilizer
Take by weighing the fertilizer sample that contains the about 100-200mg of water-soluble potassium with ten thousand/electronic balance, weigh precisely to 0.0001g, place the 250ml volumetric flask, add 150ml distilled water, shaking volumetric flask makes sample dispersion in solution, volumetric flask is placed the aqueous solution in the ultrasonic cleaner rinse bath, open ultrasonic cleaner, carry out 5 minutes ultrasonic extraction.
By above-mentioned steps, same sample carries out parallel sample operation experiments under the same conditions.Now the test data with experimental record test data and GB extracting method compares, correlation data such as following table.
The test data of table 2 ultrasonic extraction water-soluble potassium and the test data contrast table of national standard method
From above-mentioned test-results, ultrasonic extraction extracts the replicate(determination) result of potassium, and its absolute value of the bias is less than 0.14%, same sample revision test measurement result, and its absolute value of the bias meets requirement of experiment less than 0.10%; Compare with the former method of GB8574-2002, two kinds of method measurement result absolute differences meet the GB requirement less than 0.12%.But the national standard method that the time ratio of the water-soluble potassium in the ultrasonic extraction fertilizer is now carried out has shortened 12 times, and promptly 60 minute extraction time by national standard method shortens to 5 minutes.This shows the requirement that the method for the water-soluble potassium in the ultrasonic extraction fertilizer can not only satisfy rapid detection, reduce cost, and detected result accuracy height, meet the GB requirement, effectively improved the extraction efficiency of water-soluble potassium in the fertilizer.
Embodiment three
The extraction experimental implementation of available phosphorus is as follows in the fertilizer:
1. extracting solution preparation
EDTA solution claims disodium EDTA solution again, is to take by weighing 30g to 60g disodium EDTA in the 1000ml beaker, add a small amount of dissolved in distilled water,, mix to 1000ml with distilled water diluting, be mixed with the EDTA solution of concentration between 30g/L to 60g/L scope.The effect of EDTA solution is to be used for extracting available phosphorus.Phosphorus divides three kinds of forms: water-soluble phosphorus, citric acid soluble phosphorus and insoluble phosphorus, available phosphorus comprise water-soluble phosphorus and citric acid soluble phosphorus, and EDTA solution is to be used for extracting citric acid soluble phosphorus.High more when containing citric acid soluble phosphorus, the amount of then required EDTA solution is also many more, at this moment, or improves concentration, or increases consumption, seeks best joint at the two.Concentration through experimental verification EDTA solution is that the 37.5g/L extraction effect is better.When not using EDTA solution, the measurement result of phosphorus can be on the low side, because the citric acid soluble phosphorus in the fertilizer is not extracted out.
2. sampling
With sample to be extracted with the slot type reduction device through repeatedly taking out about 100g after the division, with pulverizer sample is crushed to all by the 0.5mm aperture sieve, mix, place cleaning, exsiccant weighing bottle.
3. available phosphorus in the ultrasonic extraction fertilizer
Take by weighing the fertilizer sample that contains the about 100-200mg of available phosphorus with ten thousand/electronic balance, weigh precisely to 0.0001g, place the 250ml volumetric flask, the EDTA solution that adds 150ml, shaking volumetric flask is scattered in the solution sample, volumetric flask is placed the aqueous solution in the ultrasonic cleaner rinse bath, open ultrasonic cleaner, carry out 3-15 minute ultrasonic extraction.Find that through experiment the best ultrasonic extraction time is 5 minutes.
By above-mentioned steps, same sample carries out parallel sample operation experiments under the same conditions.
Embodiment four
The extraction experimental implementation of available phosphorus is as follows in the fertilizer:
1. extracting solution preparation
Neutral ammonium citrate solution, be that dissolving 370g citric acid is in 1500ml water, add 345ml concentration and be 35.28% analytical pure ammoniacal liquor, make solution near neutral, cooling is with the pH value of acidometer mensuration solution, with (1+7) ammonia soln or citric acid solution (20g/L) regulator solution pH=7.0, thin up is to 2000ml, and solution is stored in the encloses container stand-by.
2. sampling
With sample to be extracted with the slot type reduction device through repeatedly taking out about 100g after the division, with pulverizer sample is crushed to all by the 0.5mm aperture sieve, mix, place cleaning, exsiccant weighing bottle.
3. available phosphorus in the ultrasonic extraction fertilizer
Take by weighing the fertilizer sample that contains the about 100-200mg of available phosphorus with ten thousand/electronic balance, weigh precisely to 0.0001g, place the 250ml volumetric flask, the neutral ammonium citrate solution that adds 150ml, shaking volumetric flask is scattered in the solution sample, volumetric flask is placed the aqueous solution in the ultrasonic cleaner rinse bath, open ultrasonic cleaner, carry out 3-15 minute ultrasonic extraction.Find that through experiment the best ultrasonic extraction time is 5 minutes.
By above-mentioned steps, same sample carries out parallel sample operation experiments under the same conditions.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change and revise above-mentioned embodiment.Therefore, the embodiment that discloses and describe above the present invention is not limited to also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although used some specific terms in this specification sheets, these terms do not constitute any restriction to the present invention just for convenience of description.
Claims (10)
1. the extracting method of available phosphorus, water-soluble potassium in the fertilizer is characterized in that comprising the following steps:
The preparation testing sample;
Take by weighing testing sample and be placed in the volumetric flask, add extracting solution and mix, place ultrasonic equipment to carry out ultrasonic cavitation in volumetric flask and extract.
2. the extracting method of available phosphorus, water-soluble potassium in the fertilizer according to claim 1 is characterized in that: the time that described ultrasonic cavitation extracts is 3 to 15 minutes; Described ultrasonic cavitation extracts employed ultrasonic frequency in 30KHz to 100KHz scope.
3. the extracting method of available phosphorus, water-soluble potassium in the fertilizer according to claim 2 is characterized in that: the Best Times that described ultrasonic cavitation extracts is 5 minutes; It is 60KHz that described ultrasonic cavitation extracts employed best ultrasonic frequency.
4. according to the extracting method of available phosphorus, water-soluble potassium in claim 1, the 2 or 3 described fertilizer, it is characterized in that: in the extraction of available phosphorus, described extracting solution is salpeter solution, disodium EDTA (EDTA) solution or neutral ammonium citrate solution.
5. the extracting method of available phosphorus, water-soluble potassium in the fertilizer according to claim 4 is characterized in that: the preparation composition of described salpeter solution is nitric acid and distilled water, and described salpeter solution concentration range is between (1+1) to (1+4); Described disodium EDTA (EDTA) strength of solution scope is between 30g/L to 60g/L; The preparation composition of described neutral ammonium citrate solution is citric acid and ammoniacal liquor.
6. the extracting method of available phosphorus, water-soluble potassium in the fertilizer according to claim 5 is characterized in that: the best compound concentration of described salpeter solution is (1+2); The best compound concentration of described EDTA solution is 37.5g/L.
7. according to the extracting method of available phosphorus, water-soluble potassium in claim 1, the 2 or 3 described fertilizer, it is characterized in that: in the extraction of water-soluble potassium, described extracting solution is a distilled water.
8. according to the extracting method of available phosphorus, water-soluble potassium in claim 1, the 2 or 3 described fertilizer, it is characterized in that: described ultrasonic equipment is a groove type ultrasonic ripple cleanser, and described volumetric flask is to place the aqueous solution in the ultrasonic cleaner rinse bath to carry out the ultrasonic cavitation extraction.
9. according to the extracting method of available phosphorus, water-soluble potassium in claim 1, the 2 or 3 described fertilizer, it is characterized in that: described preparation testing sample is meant sample with the slot type reduction device and is crushed to all by the 0.5mm aperture sieve with pulverizer through repeatedly taking out after the division again.
10. according to the extracting method of available phosphorus, water-soluble potassium in claim 1, the 2 or 3 described fertilizer, it is characterized in that: described what take by weighing that testing sample uses is ten thousand/electronic balance.
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| CN2010101751067A CN102001868A (en) | 2009-12-19 | 2010-05-05 | Extraction method of available phosphorus and water soluble potassium in fertilizer |
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| CN200910262298.2 | 2009-12-19 | ||
| CN2010101751067A CN102001868A (en) | 2009-12-19 | 2010-05-05 | Extraction method of available phosphorus and water soluble potassium in fertilizer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102603367A (en) * | 2012-03-05 | 2012-07-25 | 华南农业大学 | Physical and chemical comprehensive release promotion method of non-water-soluble potassium ore |
| CN110554025A (en) * | 2019-08-30 | 2019-12-10 | 内蒙古路易精普检测科技有限公司 | Method for measuring contents of water-soluble phosphorus and available phosphorus in monoammonium phosphate and diammonium phosphate by ICP method |
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| CN101082588A (en) * | 2006-06-02 | 2007-12-05 | 汤新华 | Method for rapid detecting chemical fertillizers effective phosphorus content |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102603367A (en) * | 2012-03-05 | 2012-07-25 | 华南农业大学 | Physical and chemical comprehensive release promotion method of non-water-soluble potassium ore |
| CN102603367B (en) * | 2012-03-05 | 2013-12-25 | 华南农业大学 | Physical and chemical comprehensive release promotion method of non-water-soluble potassium ore |
| CN110554025A (en) * | 2019-08-30 | 2019-12-10 | 内蒙古路易精普检测科技有限公司 | Method for measuring contents of water-soluble phosphorus and available phosphorus in monoammonium phosphate and diammonium phosphate by ICP method |
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Effective date of registration: 20110706 Address after: 518105 third industrial zone, riverside, Songgang street, Shenzhen, Guangdong, Baoan District Applicant after: Batian Ecological Engineering Co., Ltd., Shenzhen Co-applicant after: Xuzhou Batian Ecology Co., Ltd. Address before: 518105 third industrial zone, riverside, Songgang street, Shenzhen, Guangdong, Baoan District Applicant before: Batian Ecological Engineering Co., Ltd., Shenzhen |
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