CN109490032A - A kind of sample-pretreating method measuring corn silage ammonia nitrogen content - Google Patents
A kind of sample-pretreating method measuring corn silage ammonia nitrogen content Download PDFInfo
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- CN109490032A CN109490032A CN201811295583.XA CN201811295583A CN109490032A CN 109490032 A CN109490032 A CN 109490032A CN 201811295583 A CN201811295583 A CN 201811295583A CN 109490032 A CN109490032 A CN 109490032A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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Abstract
The invention belongs to agricultural product storage technique field more particularly to a kind of sample-pretreating methods for measuring corn silage ammonia nitrogen content, are used as sample specifically includes the following steps: the corn silage of acquisition is mixed；20g ensiling sample is accurately weighed, is placed in the glass beaker of 500ml；180ml distilled water is added, stands 30min under room temperature after stirring 1min, filters；Measure the ammonia nitrogen content of leaching liquor.Accuracy of measurement of the present invention is high, and the standard deviation of 3 repeat samples is within 0.23%.Extracting solution is distilled water, is easier to obtain relative to deionized water and ultrapure water.Extraction temperature is room temperature, can reduce the requirement during extracting to temperature environment.Determine extraction concentration, i.e. 20g ensiling sample extracts in 180ml distilled water.Extraction time is 30min, and the time is shorter, has been obviously shortened extraction time for 24 hours relative to currently used extraction.
Description
Technical field
The invention belongs to agricultural product storage technique field more particularly to a kind of samples for measuring corn silage ammonia nitrogen content
Pre-treating method.
Background technique
Currently, the prior art commonly used in the trade is such that
Ensilage is one of the main roughage of ruminant cultivation.Whole corn silage is high with its nutritive value, protects
The advantages that effect is good is deposited, the 30%~80% of roughage ratio is accounted in milk cow diet recipe.Currently, ensilage also gradually exists
It is widely applied in beef cattle and mutton sheep diet.Since 2015, " grain changes feeding " policy that country puts into effect was written into for continuous 3 years
Entreat No.1 file." grain changes feeding ", which mainly takes, pushes agricultural structure adjustment in a manner of feeding band kind, promotes silage corn, clover, swallow
The plantation of the forage crops such as wheat, sorghum saccharatum and beans, this will further improve the application range and usage amount of ensilage.Ensiling is raised
The value of material depends primarily on the nutritive value of raw material and the quality of fermentation quality.
Ammoniacal nitrogen (NH3- N) account for the ratio (NH of total nitrogen (TN)3- N/TN) it is the key that evaluation ensilage fermentation quality refers to
Mark.Evaluate NH3The premise of-N/TN ratio is the NH for measuring ensilage3N content and TN content.It as former state can with ensilage
To measure TN content, and measure NH3N content needs to carry out extraction processing to sample, then measures the NH of leaching liquor3N content, and
The NH of ensilage is represented with this3N content.Nearly 10 years, NH is measured in research and production3To the preceding place of sample when N content
It is larger to manage (extraction) method divergence, be mainly manifested in ensilage extraction concentration in the solution, time, temperature and extracts molten
Four aspects of type of liquid；As the ratio of ensilage fresh weight and leaching liquor has 1:9,1:5,1:4,1:2；Ensilage is in solution
In extraction time have extraction for 24 hours, 18h, 1h, 30min, 5min；Extraction temperature has 4 DEG C, 5 DEG C, 30 DEG C, room temperature；Extracting solution
There are distilled water, deionized water and ultrapure water.These different sample-pretreating methods make ensiling sample measurement result inaccuracy,
Sample pretreatment process is cumbersome, the comparativity between different measurement results is poor.
In conclusion problem of the existing technology is: measuring NH in the prior art3To the pre-treatment of sample when N content
(extraction) method divergence is larger, and different sample-pretreating methods makes measurement result inaccuracy, the sample pre-treatments of ensiling sample
Process is cumbersome, the comparativity between the measurement result of different experiments room is poor.
Solve the difficulty and meaning of above-mentioned technical problem:
The difficulty for solving above-mentioned technical problem is the difference between more existing several major sample pre-treating methods,
And filter out reproducible and easy pre-treating method.
Unified measuring method can reduce the difference of measurement result between different experiments room, improve the accuracy of measurement result,
And simplify sample pretreatment process.
Summary of the invention
In view of the problems of the existing technology, the present invention provides before a kind of sample for measuring corn silage ammonia nitrogen content
Processing method.
The invention is realized in this way a kind of sample-pretreating method for measuring corn silage ammonia nitrogen content, specific to wrap
Include following steps:
Step 1: the corn silage of acquisition is reduced to about 5kg with quartering, and is mixed as test specimen；
Step 2: 20g ensiling sample is accurately weighed, is placed in the glass beaker of 500ml；
Step 3: being added 180ml distilled water, stands 30min under room temperature after stirring 1min, filters；
Step 4: with the ammoniacal nitrogen NH of spectrophotometric determination leaching liquor3N content replication 3 times, is averaged.
Further, precise 20g sample, is accurate to 0.1g.
Further, NH is surveyed using phenol-sodium hypochlorite colorimetric method3N content, and calculate NH3The ratio of-N/TN.
Further, room temperature condition are as follows: 11-18 DEG C.
Further, the ammoniacal nitrogen NH of spectrophotometric determination leaching liquor is used after filtering3N content replication 3 times, is put down
Mean value is just the ammoniacal nitrogen NH of the sample3N content.
In conclusion advantages of the present invention and good effect are as follows: the present invention is handled under the conditions of comparing different temperatures, time etc.
The ammonia nitrogen content of ensilage sample have indifference, if indifference, we just may be selected the shortest time, are easiest to obtain
Temperature (room temperature) under the conditions of handle ensilage sample, and for measuring ammonia nitrogen content.Accuracy of measurement of the present invention is high,
The standard deviation of 3 repeat samples is within 0.23%.Extracting solution is distilled water, is easier to obtain relative to deionized water and ultrapure water
?.Extraction temperature is room temperature, reduces the requirement during extracting to temperature environment.Determine extraction concentration, i.e. 20g ensiling sample exists
It is extracted in 180ml distilled water.Extraction time is 30min, and the time is shorter, relative to being obviously shortened extraction time for 24 hours.The present invention
Ammonia nitrogen content for quick Accurate Determining ensilage.Ammonia nitrogen content is albumen during evaluation ensilage fermentation
The most important index of matter palliating degradation degree.Protein degradation amount is bigger, and the fermentation quality for illustrating ensilage is poorer.
Detailed description of the invention
Fig. 1 is the sample-pretreating method flow chart of measurement corn silage ammonia nitrogen content provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Carry out sample-pretreating method pair in terms of leaching liquor type, leaching liquor concentration, extraction time, extraction temperature four
Ensilage NH3The comparison that N content influences proposes the sample-pretreating method of measurement corn silage ammonia nitrogen content.
Application principle of the invention is described in detail with reference to the accompanying drawing.
As shown in Figure 1, the sample-pretreating method of measurement corn silage ammonia nitrogen content provided in an embodiment of the present invention, tool
Body the following steps are included:
S101: the corn silage of acquisition is reduced to about 5kg with quartering, and is mixed as test specimen；
S102: 20g ensiling sample is accurately weighed, is placed in the glass beaker of 500ml；
S103: being added 180ml distilled water, stands 30min under room temperature after stirring 1min, filters；
S104: with the ammoniacal nitrogen NH of spectrophotometric determination leaching liquor3N content replication 3 times, is averaged.
Precise 20g sample provided in an embodiment of the present invention, is accurate to 0.1g.
It is provided in an embodiment of the present invention that ammoniacal nitrogen NH is surveyed using phenol-sodium hypochlorite colorimetric method3N content, and calculate NH3-
The ratio of N/TN.
Room temperature condition provided in an embodiment of the present invention are as follows: 11-18 DEG C.
The ammoniacal nitrogen NH of measurement leaching liquor provided in an embodiment of the present invention3N content, replication 3 times, average value is just
For the ammoniacal nitrogen NH of the sample3N content.
Very thin explanation is made to application principle of the invention below with reference to specific experiment；
Experiment 1；
1, experiment specifically includes following four part:
(1) extracting solution is to ensiling NH3The influence of N content
It is designed using single factor experiment, 36 parts of sample of precise 20g (being accurate to 0.1g) is individually positioned in the glass of 500ml
In glass beaker, it is separately added into 180ml distilled water, deionized water and ultrapure water in 12 parts of samples wherein at random, at room temperature
Ammoniacal nitrogen NH is measured immediately after (11-18 DEG C) extraction for 24 hours3N content.
(2) extraction concentration is to ensiling ammoniacal nitrogen NH3The influence of N content
It is designed using single factor experiment, 36 parts of sample of precise 20g (being accurate to 0.1g) is individually positioned in the glass of 500ml
In glass beaker, 90,180,270ml distilled water are separately added into 12 parts of samples wherein at random, at room temperature (11-18 DEG C) leaching
Ammoniacal nitrogen NH is measured after mentioning for 24 hours immediately3N content.
(3) extraction temperature is to ensiling NH3The influence of N content
It is designed using single factor experiment, 36 parts of sample of precise 20g (being accurate to 0.1g) is individually positioned in the glass of 500ml
In glass beaker, 180ml distilled water is added and is sealed with preservative film.Wherein 12 parts of samples are individually positioned in 4 DEG C of refrigerators, 30 at random
Ammoniacal nitrogen NH is measured immediately after extracting for 24 hours in DEG C insulating box and room temperature (11-18 DEG C) environment3N content.
(4) extraction time is to ensiling ammoniacal nitrogen NH3The influence of N content
It is designed using single factor experiment, 12 parts of sample of precise 20g (being accurate to 0.1g) is individually positioned in the glass of 500ml
In glass beaker, be added 180ml distilled water, at room temperature (11-18 DEG C) extracted respectively to 30min, 12h, for 24 hours with measurement when 48h
The ammoniacal nitrogen NH of 12 parts of samples3N content.
Ammoniacal nitrogen NH is surveyed using phenol-sodium hypochlorite colorimetric method3N content, and calculate NH3The ratio of-N/TN.Each sample
3 repetitions of product.
2, result；
As shown in table 1, sample-pretreating method is to corn silage NH3The influence result of-N/TN ratio.
The NH of the type of extracting solution and extraction temperature in distilled water to ensiling3- N/TN ratio is all without significant shadow
It rings (P > 0.05).20g ensiling extracted for 24 hours in 90,180,270ml distilled water after NH3- N/TN ratio is respectively 5.62%,
4.22%, 3.15%, significant difference (P < 0.05).With the extension of extraction time, the NH of ensiling3- N/TN ratio linearly increases
(P < 0.05) extracts the NH of 48h3- N/TN ratio and extraction are not significantly different (P > 0.05) for 24 hours, but are significantly higher than extraction 12h
With the NH of 30min3- N/TN ratio (P < 0.05)；The NH of extraction for 24 hours3- N/TN ratio is significantly higher than the NH of extraction 30min3-N/TN
Ratio (P < 0.05).
1 sample-pretreating method of table is to corn silage NH3The influence of-N/TN ratio, %
In conclusion the sample-pretreating method of the ensilage ammoniacal nitrogen measurement determined in the present invention are as follows: accurately weigh
20g ensiling sample, is placed in the glass beaker of 500ml, and 180ml distilled water is added, and stands under room temperature after stirring 1min
30min uses the ammonia nitrogen content of spectrophotometric determination leaching liquor after filtering, replication 3 times, average value is just the sample
Ammonia nitrogen content.
Accuracy of measurement of the present invention is high, and the standard deviation of 3 repeat samples is within 0.23%.Extracting solution is distilled water,
It is easier to obtain relative to deionized water and ultrapure water.Extraction temperature is room temperature, reduces the requirement during extracting to temperature environment.Really
Surely concentration is extracted, i.e. 20g ensiling sample extracts in 180ml distilled water.Extraction time is 30 minutes, and the time is shorter, relative to
Currently used extraction has been obviously shortened extraction time for 24 hours.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (5)
1. a kind of sample-pretreating method for measuring corn silage ammonia nitrogen content, which is characterized in that the measurement corn silage
The sample-pretreating method of ammonia nitrogen content the following steps are included:
Step 1: the corn silage of acquisition is reduced to 5kg with quartering；
Step 2: 20g ensiling sample is weighed, is placed in the glass beaker of 500ml；
Step 3: being added 180ml distilled water, stands 30min under room temperature after stirring 1min, filters；
Step 4: it with the ammonia nitrogen content of spectrophotometric determination leaching liquor, replication 3 times, is averaged.
2. the sample-pretreating method of measurement corn silage ammonia nitrogen content as described in claim 1, which is characterized in that described
Ammoniacal nitrogen NH is surveyed using phenol-sodium hypochlorite colorimetric method3N content, and calculate ammoniacal nitrogen NH3- N accounts for the ratio NH of total nitrogen TN3-
N/TN。
3. the sample-pretreating method of measurement corn silage ammonia nitrogen content as described in claim 1, which is characterized in that described
Room temperature condition are as follows: 11-18 DEG C.
4. the sample-pretreating method of measurement corn silage ammonia nitrogen content as described in claim 1, which is characterized in that described
The ammonia nitrogen content of spectrophotometric determination leaching liquor is used after filtering, replication 3 times, average value is the ammoniacal nitrogen of the sample
Content.
5. a kind of using the sample-pretreating method for measuring corn silage ammonia nitrogen content described in Claims 1 to 4 any one
Ensilage ammonia nitrogen content measure system.
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| CN102524527A (en) * | 2012-02-13 | 2012-07-04 | 中国农业大学 | Chinese herbal medicine type silage biological additive and use thereof |
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| CN103843991A (en) * | 2013-12-31 | 2014-06-11 | 中国科学院地理科学与资源研究所 | Wheat straw and perennial ryegrass containing silage composition and application thereof |
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