CN103969204A - Method for rapidly detecting phosphorus in forage-grade calcium hydrogen phosphate - Google Patents
Method for rapidly detecting phosphorus in forage-grade calcium hydrogen phosphate Download PDFInfo
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- CN103969204A CN103969204A CN201410224699.XA CN201410224699A CN103969204A CN 103969204 A CN103969204 A CN 103969204A CN 201410224699 A CN201410224699 A CN 201410224699A CN 103969204 A CN103969204 A CN 103969204A
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- phosphorus
- forage
- hydrogen phosphate
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Abstract
The invention discloses a novel method for determining the content of phosphorus in forage-grade calcium hydrogen phosphate by using spectrophotometry, belonging to the technical field of quality detection of forage. The method comprises the following steps: preparing a hydrochloric acid solution and a vanadium ammonium molybdate chromogenic agent; preparing a phosphorus standard solution; building a regression equation; preparing and determining a sample. According to the method, the spectrophotometry is utilized for determining the content of phosphorus in forage-grade calcium hydrogen phosphate, the accuracy and the precision are high, and the used agent is safe. Compared with a quinolone-sodium molybdate-citric acid-acetone weight method in GB/T22549-2008 Forage-grade Calcium Hydrogen Phosphate, the method is relatively simple, convenient and fast.
Description
Technical field
The present invention relates to measure in field of fodder the method for calcium monohydrogen phosphate, relate in particular to a kind of detection method of measuring Phosphorus Contents in Calcium Hydrogen Phosphate.
Background technology
In present GB/T22549-2008 " calcium hydrophosphate fodder ", the method that detects Phosphorus Contents in Calcium Hydrogen Phosphate content is gravimetric method, detects principle to be: in acid solution, phosphate radical all forms deposit with the quinoline molybdenum lemon ketone precipitation agent adding, by filtering, dry, weighing, calculate phosphorus content.By the content of gravimetric determination phosphorus, method maturation, result is accurate, but complex operation, time-consuming (more than 3h), and in quinoline molybdenum lemon ketone precipitation agent, quinoline (C
9h
7and acetone (C N)
3h
6o) be all hazardous chemical, harmful.Acetone is a kind of high molecular weight water soluble polymer, has moderate toxicity, can be used as the raw material of producing methamphetamine, belongs to control chemicals, and acetone can be absorbed by the body through respiratory tract, alimentary canal and skin, can cause poisoning in the situation that contact is more.Detect the content of Phosphorus Contents in Calcium Hydrogen Phosphate by gravimetric method, can not adapt in actual applications produce and the simple and direct and safe requirement of scientific research to analytical work, therefore, need a kind of quick and safe method to substitute.
At present, in Feed Manufacturing and inspection, GB/T6437-2002 " mensuration of total phosphorus in feed " uses the content of the phosphorus in Feed by Spectrophotometry.Its principle is: first the organism in Feed Sample is destroyed, the phosphorus in feed is dissociated out, use vanadium ammonium molybdate processing in acid solution, generate yellow phosphorus molybdenum Huang [(NH
4)
3pO
4nH
4vO
316M
0o
3], in wavelength 420nm place's colorimetric estimation.
Compared with the gravimetric method of GB/T22549-2008 " calcium hydrophosphate fodder ", spectrophotometric method is very simple and convenient, if be used in the mensuration of the phosphorus content in calcium monohydrogen phosphate, will give and produce and inspection work bring great convenience.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, and a kind of detection method of applying spectrophotometric method is provided.
For solving the problems of the technologies described above, technical scheme of the present invention comprises step: preparation developer, determine test condition, Criterion curve.
Preparation developer takes analyzes pure ammonium metavanadate 1.25g, and adding distil water 200mL heating for dissolving, adds 250mL to analyze pure nitric acid after cooling again.Separately take and analyze pure ammonium molybdate 25g, adding distil water 400mL heating for dissolving.After cooling, 2 kinds of solution are mixed, be settled to 1L with distilled water.The precipitation of generation keeps in Dark Place, if can not continue to use.
Determine that test condition developer adds 10mL, under normal temperature, more than standing 10min, measuring wavelength is 420nm.
Criterion curve pipettes respectively phosphorus standard solution 0,1,2,4,6,8,10,12mL in 50mL volumetric flask, respectively add vanadium ammonium molybdate developer 10mL, with distilled water diluting to scale, shake up, more than placing 10min under normal temperature, taking 0mL phosphorus standard solution as reference, by 1cm cuvette absorbance with the each solution of spectrophotometric determination under 420nm wavelength, measurement result is taking phosphorus concentration (ug/mL) as horizontal ordinate, absorbance is that ordinate carries out linear regression, obtains typical curve equation.
Brief description of the drawings
The accompanying drawing of this instructions is to obtain typical curve equation according to phosphorus concentration and absorbance, uses the mapping of Excel software, has reflected the relation of phosphorus concentration and absorbance.
Embodiment
Instrument and equipment FA1104N electronic balance (Shanghai Precision Scientific Apparatus Co., Ltd): sensibility reciprocal 0.0001g.752N ultraviolet-visible pectrophotometer (Shanghai Precision Scientific Apparatus Co., Ltd): can measure at 420nm place absorbance.Cuvette: 1cm.50,100,1000mL volumetric flask:.1,2,3,5,10mL transfer pipet:.25,500,1000mL beaker:.Temp. controllable electric furnace: 1KW.Digital display electric drying oven with forced convection (PVG Rong Feng scientific instrument company limited): 50～300 DEG C.
Preparation hydrochloric acid solution: will analyze 1: 3 by volume preparation hydrochloric acid solution of pure hydrochloric acid and distilled water.
Preparation developer: take and analyze pure ammonium metavanadate 1.25g, adding distil water 200mL heating for dissolving, adds 250mL to analyze pure nitric acid after cooling again.Separately take and analyze pure ammonium molybdate 25g, adding distil water 400mL heating for dissolving.After cooling, 2 kinds of solution are mixed, be settled to 1L with distilled water.The precipitation of generation keeps in Dark Place, if can not continue to use.
Preparation phosphorus titer: will analyze pure phosphoric acid potassium dihydrogen at 105 DEG C of dry 1h, and take 0.2195g after cooling in exsiccator and be dissolved in distilled water, and quantitatively proceed in 1L volumetric flask, add and analyze pure nitric acid 3mL,, shake up to scale with distilled water diluting, be the phosphorus titer of 50ug/mL.
Criterion curve: pipette respectively phosphorus standard solution 0,1,2,4,6,8,10,12mL in 50mL volumetric flask, respectively add vanadium ammonium molybdate developer 10mL, with distilled water diluting to scale, shake up, more than placing 10min under normal temperature, taking 0mL phosphorus standard solution as reference, by 1cm cuvette absorbance with the each solution of spectrophotometric determination under 420nm wavelength, measurement result is taking phosphorus concentration (ug/mL) as horizontal ordinate, absorbance is that ordinate carries out linear regression, obtains typical curve equation y=0.0508x+0.0793 (R
2=0.9995) (table 1).
The relation of table 1 phosphorus concentration and absorbance
Sample preparation takes 0.1g left and right calcium hydrophosphate fodder sample and is placed in 25mL beaker, adds 10mL dissolve with hydrochloric acid solution, moves in 100mL volumetric flask, is diluted with water to scale
Sample determination pipettes sample decomposed solution 1mL in 50mL volumetric flask, add vanadium ammonium molybdate developer 10mL, be diluted with water to scale, shake up, more than placing 10min under normal temperature, measure at 420nm wavelength place with 1cm cuvette, by above-mentioned the absorbance substitution of the sample decomposed solution reading typical curve equation, obtain nitrite ion concentration (ug/mL) and be calculated as follows again the phosphorus content in sample calcium hydrophosphate fodder.
P＝C×V×D×0.0001/m
In formula: P is phosphorus content (%); The nitrite ion phosphorus concentration (ug/mL) of C for being tried to achieve by typical curve equation (y=0.0508x+0.0793); V is color volume, 50mL; D gets multiple (constant volume: divide and get volume, 100: 1) for dividing; 0.0001 refers to the factor that ug/g is scaled to percentage composition.
Results and analysis
Precision test takes respectively about 0.1g and analyzes No. 1, pure phosphoric acid hydrogen calcium and analyze each 6 of No. 2, pure phosphoric acid hydrogen calcium, in the time setting up with typical curve, under identical experiment condition, measures, and result is as shown in table 2.The molecular formula of sample analysis pure phosphoric acid hydrogen calcium is CaHPO
42H
2o, the theoretical value of phosphorus content is 18.02%.From table 2,2 measured values of analyzing pure phosphoric acid hydrogen calcium samples are all approaching with theoretical value, and the coefficient of variation is less than 0.3%, illustrate that the method precision is high.
Table 2 Precision test result
Accuracy test is in order directly to illustrate the difference between spectrophotometric method and GB/T22549-2008 " calcium hydrophosphate fodder " method (National Standard Method), apply respectively these 2 kinds of methods and measure 4 calcium hydrophosphate fodder sample phosphorus contents, to each sample replication 6 times, its mean value the results are shown in Table 3.From table 3, the absolute difference of each measurement result and mean value is all less than 0.2%.In National Standard Method, specify, phosphorus content >=16.5% in calcium hydrophosphate fodder, as can be seen from Table 3, the absolute difference of spectrophotometric method and National Standard Method is 0.09%～0.16%, all be less than 2 replicate determination result absolute differences that allow in National Standard Method and be not more than 0.2%, relative error is 0.53%～0.95%, and relative error is less than 1%, illustrates that spectrophotometric method accurately, reliably.
Table 3 accuracy test result
Compared with prior art GB/T22549-2008 " calcium hydrophosphate fodder ", the invention has the advantages that:
With the phosphorus content in Feed by Spectrophotometry calcium hydrophosphate, easy, accurate, greatly shortened the time compared with gravimetric method, agents useful for same safety can be applicable in real work.
Claims (3)
1. a method for quick of measuring the phosphorus content in calcium hydrophosphate fodder, is characterized in that, the phosphorus content in application Feed by Spectrophotometry level acid hydrogen calcium.
2. according to the method described in claims 1, it is characterized in that, described condition determination is: developer adds 10mL, and under normal temperature, more than standing 10min, measuring wavelength is 420nm.
3. according to the method described in claims 1, it is characterized in that, described method adopts typical curve to carry out quantitative test to sample, and for measuring the phosphorus content of calcium hydrophosphate fodder.
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| CN201410224699.XA CN103969204A (en) | 2014-05-22 | 2014-05-22 | Method for rapidly detecting phosphorus in forage-grade calcium hydrogen phosphate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187520A (en) * | 2018-08-22 | 2019-01-11 | 漳州傲农牧业科技有限公司 | A kind of method of citric acid soluble phosphorus in quick measurement feedstuff calcium monohydrogen phosphate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101788494A (en) * | 2010-01-29 | 2010-07-28 | 迁安市津唐球墨铸管有限公司 | Method for measuring phosphorous content by adopting bismuth phosphomolybdate blue-sulfuric acid photometry |
| CN102393368A (en) * | 2011-10-28 | 2012-03-28 | 内蒙古包钢钢联股份有限公司 | Method for measuring phosphorus content in sponge iron |
| CN102539426A (en) * | 2012-01-06 | 2012-07-04 | 吉林建龙钢铁有限责任公司 | Method for determining phosphorus in silicon-manganese alloy |
| CN102928371A (en) * | 2012-11-08 | 2013-02-13 | 成武县农业局 | Method for rapidly determining available phosphorus content in compound fertilizer through spectrophotometer |
| CN102998266A (en) * | 2012-11-21 | 2013-03-27 | 合肥星宇化学有限责任公司 | Method for analyzing total phosphorus in industrial sewage sample |
-
2014
- 2014-05-22 CN CN201410224699.XA patent/CN103969204A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101788494A (en) * | 2010-01-29 | 2010-07-28 | 迁安市津唐球墨铸管有限公司 | Method for measuring phosphorous content by adopting bismuth phosphomolybdate blue-sulfuric acid photometry |
| CN102393368A (en) * | 2011-10-28 | 2012-03-28 | 内蒙古包钢钢联股份有限公司 | Method for measuring phosphorus content in sponge iron |
| CN102539426A (en) * | 2012-01-06 | 2012-07-04 | 吉林建龙钢铁有限责任公司 | Method for determining phosphorus in silicon-manganese alloy |
| CN102928371A (en) * | 2012-11-08 | 2013-02-13 | 成武县农业局 | Method for rapidly determining available phosphorus content in compound fertilizer through spectrophotometer |
| CN102998266A (en) * | 2012-11-21 | 2013-03-27 | 合肥星宇化学有限责任公司 | Method for analyzing total phosphorus in industrial sewage sample |
Non-Patent Citations (3)
| Title |
|---|
| 毛艳贞等: "分光光度法测定饲料级磷酸盐中总磷含量", 《饲料研究》 * |
| 申爱华等: "分光光度法测定饲料级磷酸氢钙中磷的含量", 《江苏农业科学》 * |
| 金善玉等: "分光光度法在分析饲料级磷酸氢钙过程中的应用", 《水产科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187520A (en) * | 2018-08-22 | 2019-01-11 | 漳州傲农牧业科技有限公司 | A kind of method of citric acid soluble phosphorus in quick measurement feedstuff calcium monohydrogen phosphate |
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Application publication date: 20140806 |