CN104931437A - Method for detecting contents of potassium, calcium and magnesium in plant - Google Patents
Method for detecting contents of potassium, calcium and magnesium in plant Download PDFInfo
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Abstract
The invention discloses a method for detecting the contents of potassium, calcium and magnesium in a plant. The method comprises the following steps: drying a preprocessed plant sample to constant weight at 65 to 100 DEG C, heating hydrochloric acid, mixing and oscillating, filtering to obtain filter liquor, diluting to constant volume, and detecting the contents of the potassium, the calcium and the magnesium by adopting a flame absorption method of an atomic absorption spectrophotometer. According to the method, the hydrochloric acid is heated for extracting mineral elements contained in the plant sample, and the heated hydrochloric acid also can be used for fully extracting the potassium, the calcium and the magnesium in the sample with compact structure or high grease content. The heated hydrochloric acid is capable of fully extracting screened plant sample granules, the operation is simple, the working pressure of detection personnel is reduced, and the detection method is very high in accuracy and precision for detecting the contents of the potassium, the calcium and the magnesium, safe, environment-friendly, good in detection repeatability, accurate, efficient, simple and convenient to operate and suitable for batch sample treatment.
Description
Technical field
The present invention relates to a kind of method detecting potassium, content of calcium and magnesium, particularly a kind of method detecting potassium in plant, content of calcium and magnesium.
Background technology
Plant Mineral Elements potassium, content of calcium and magnesium analysis lack diagnosis of plant nutrient is rich, understand plant growth rule, regulating plant anti-adversity ability, instruct the rational application of fertilizer and scientific management important in inhibiting (Zhou Wei, Wang Hong " BULLETIN OF BOTANY Vol. Calcium in Plants absorbs, transhipment and the physiology of metabolism and molecular mechanism " 2007,24 (6), BULLETIN OF BOTANY Vol., 762-778).The methods such as humidifying method, ashing method are mainly contained in current detection potassium of plants, content of calcium and magnesium technology.Disappear cooking method and sulfuric acid-perchloric acid of nitric acid-perchloric acid described in GB GB7857-87, forestry industry standard LY/T1237-1999 disappears cooking method, and these two kinds of methods have the defect that Digestion time is long, acid mist pollution is serious, environment and personnel health are all had to harm.In use there is potential safety hazard (Duan Duoxiu in nitric acid used, sulfuric acid and perchloric acid, Xiangdong Zhang, Hui Wen " lixiviation method and the cooking method that disappears measure the comparative studies of potassium calcium content in herbage ", 200641 (2), Gansu Agriculture University journal 65-69).Ashing method complex operation, carbonize from sample, high temperature ashing, diluted hydrochloric acid dissolution prepares the operation controls such as liquid to be measured to constant volume improper, easily occur that ashing is not thorough, element loss and Partial Elements generate the silicate of indissoluble and cause testing result (" in plant sample the sample-pretreating method of Elements and determination techniques " on the low side, Liu Yuxuan, Li Xiaojing, Bai Quanfeng, 2013 (10), rock and mineral testing, 681-693) (wear improve oneself " research that watery hydrochloric acid extraction measures mineral nutrient element in tealeaves ", Beijing Agricultural College's journal, 1999 (01)).
Current data proposes the method comparatively ashing method convenient operation that HCl extract measures potassium of plants, content of calcium and magnesium, and detection efficiency is high.This plant sample is directly added hydrochloric acid at room temperature vibrate 2 hours lixiviates measure plant sample potassium, calcium, magnesium element content method many employings plant leaf blade sample be research object (Peng Xiaoxia, Li Ke, Wu Jingke, Jiang Xiangning, " a kind of fast and convenient HCl extracts the method for Multielement Analysis in Plant Samples ", analytical instrument, 2008 (4), 19-23) (Fast Measurement forestry science and technology 200025 (2) 14-15 of Liu Xiao brightness Chen Hui Chen Zhiqiang China fir needle Mineral Elements).But be also shown in dry particle when filtering after vibrating 2 hours to the organ samples particle such as plant peel, branch that difficulty infiltrates, this situation causes testing result on the low side.Have data to propose first to infiltrate sample with hydrochloric acid, then lixiviate in 2 hours of vibrating measure the method (Wei Gang Xia Zuyan " comparison test of trees sample wet ashing technique and extraction " Beijing Forestry University's journal 1985 (04) 103-107) of potassium of plants, content of calcium and magnesium.The method with organs such as pinaceae plant sample branch, leaf, roots for sample lixiviate is abundant, but infiltrate and vibration extraction time long, detection efficiency is low, to hydrochloric acid how infiltration of plants sample method not clearly, not easily grasp.
The information being disclosed in this background technology part is only intended to increase the understanding to general background of the present invention, and should not be regarded as admitting or imply in any form that this information structure has been prior art that persons skilled in the art are known.
Summary of the invention
The object of the present invention is to provide a kind of method detecting potassium in plant, content of calcium and magnesium, thus overcome in technology today the mineral element potassium in plant, calcium, magnesium detection efficiency is not high, testing result deviation is larger shortcoming, the inventive method is simple to operate, detects precise and high efficiency.
For achieving the above object, technical scheme provided by the invention is as follows:
A kind of method detecting potassium in plant, content of calcium and magnesium, comprise following operation: dry pretreated plant sample 65 ~ 100 DEG C to constant weight, the vibration of heating mixed in hydrochloric acid, filter, get filtrate, the flame absorption process of atomic absorption spectrophotometer (AAS) is adopted to measure the content of potassium, calcium, magnesium after dilution constant volume.
Preferably, described hot hydrochloric acid refers to that temperature is the hydrochloric acid of 50 ~ 100 DEG C.
Preferably, described hot hydrochloric acid refers to that temperature is the hydrochloric acid of 50 ~ 60 DEG C.
Preferably, described hot hydrochloric acid volumetric concentration is 1mol/L.
Preferably, described 65 ~ 100 DEG C of plant samples of drying to constant weight, add the hot hydrochloric acid of 20 ~ 100ml according to the amount of every 100 ~ 400mg.
Preferably, described pre-service is that plant sample is toasted 8 ~ 48h through 60 ~ 80 DEG C, pulverizes and crosses 18 ~ 60 mesh sieves.
Preferably, described pre-service is that plant sample is toasted 8 ~ 48h through 60 ~ 80 DEG C, pulverizes and crosses 40 ~ 60 mesh sieves.
Preferably, described heating mixed in hydrochloric acid vibration 60 ~ 90min, oscillation frequency is 200Hz.
Preferably, dry the plant sample to constant weight, put into the plastic centrifuge tube with a scale of 40 ~ 100ml, heating mixed in hydrochloric acid.
Compared with prior art, the present invention has following beneficial effect:
The present invention is to heat mineral element contained by HCl extract plant sample, and the hydrochloric acid after heating is to organizing consolidation or also very good containing the Detection results after the potassium in the high sample of grease, calcium, magnesium elements lixiviate.Hydrochloric acid after heating can fully to sieve plant sample particle in lixiviate, simple to operate, alleviate testing staff's working pressure, detection method detects potassium in plant, content of calcium and magnesium accuracy rate, precision are high, safety and environmental protection, detects repeatability good, precise and high efficiency, simple to operation, be suitable for batch sample process.
Embodiment
Be described in detail below in conjunction with embodiment, but be to be understood that protection scope of the present invention not by the restriction of embodiment.In the examples below, used material and equipment as follows:
1, plant sample is (from masson pine skin, branch in the summer stone mountain artificial forest of Tropical Forest experimental center, Chinese forest-science academy; The leaf of Tokyo paulownia; The branch of red vertebra tree);
2, hydrochloric acid solution (is got 84ml concentrated hydrochloric acid (analyzing pure) dilute constant volume 1000ml with deionized water and get final product; Concentrated hydrochloric acid manufacturing enterprise: Chengdu Ke Long chemical reagent factory, buys in Nanning Hui Xinhua glass Instrument Ltd.);
3, massfraction is that 5% lanthanum chloride solution (takes 5g lanthanum chloride (analyzing pure) to be dissolved in deionized water and to be settled to 100ml, to obtain final product; Lanthanum chloride manufacturing enterprise: Chemical Reagent Co., Ltd., Sinopharm Group, buys in Nanning Hui Xinhua glass Instrument Ltd.);
4,20 μ g/ml potassium mark liquid (take the potassium chloride (analyzing pure) that 0.1907g is dried through 105 DEG C, be dissolved in deionized water, add the obtained 100 μ g/ml potassium mark liquid of 10ml concentrated hydrochloric acid constant volume 1000ml, extract 20ml, with obtained 20 μ g/ml potassium mark liquid after deionized water dilution constant volume 100ml; KCl production enterprise: Dihua work stock is won from company limited in Tianjin, buys in Nanning Hui Xinhua glass Instrument Ltd.);
5,100 μ g/ml calcium mark liquid: take the calcium carbonate (top grade is pure) that 2.4970g is dried through 105 DEG C, with adding 100ml deionized water and 10ml concentrated hydrochloric acid after 0.2mol/L dissolving with hydrochloric acid, obtain the calcium mark liquid of 1000 μ g/ml to 1000ml with deionized water constant volume, extraction 10ml dilution is settled to 100ml and namely obtains 100 μ g/ml calcium mark liquid; Calcium carbonate manufacturing enterprise: Tianjin Ke Miou chemical reagent company limited, buys in Nanning Hui Xinhua glass Instrument Ltd.);
6,20 μ g/ml magnesium mark liquid: take the magnesium oxide (top grade is pure) that 0.1658g is dried through 105 DEG C, with adding 200ml deionized water and 10ml concentrated hydrochloric acid after 1:3 dissolving with hydrochloric acid, obtain the magnesium mark liquid of 100 μ g/ml with deionized water constant volume to 1000ml, extract 20ml dilute with water constant volume 100ml and namely obtain 20 μ g/ml magnesium mark liquid; Magnesium oxide manufacturing enterprise: Dihua work stock is won from company limited in Tianjin, buys in Nanning Hui Xinhua glass Instrument Ltd.);
7, electronic balance;
8, baking oven;
9, oscillator;
10, atomic absorption spectrophotometer (AAS) (TAS-999);
11, muffle furnace.
Embodiment 1
Get 500g plant sample Tokyo paulownia leaf be placed in baking oven keep temperature be 60 DEG C baking 30h, take out and pulverize, dry to constant weight at 100 DEG C again after crossing 18 mesh sieves, for subsequent use, get 250mg plant sample for subsequent use, put into the plastic centrifuge tube with a scale of 100ml, add the hot mixed in hydrochloric acid of 100ml 1mol/L of 60 DEG C, capping, with 200Hz hunting of frequency 60min, filter with quantitative filter paper, filter and terminate, extract filtrate 2ml, the lanthanum chloride 0.5ml of 5%, put into the volumetric flask of 25ml, be settled to 25ml with deionized water, shake up.Plant sample repeats 3 times as stated above, and the work not adding sample is blank, repeats 3 times with said method.Extract 20 μ g/ml potassium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the potassium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml.Detect potassium with atomic absorption spectrophotometer (AAS), average.Extract 100 μ g/ml calcium mark liquid 0,0.5,1,2,4ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the standard calcium serial solution of 0,2,4,8,16 μ g/ml.Calcium content is detected with atomic absorption spectrophotometer (AAS).Extract 20 μ g/ml magnesium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, the blank 2ml of each extraction, 5% lanthanum chloride 0.5ml add, add deionized water again to scale, obtain the magnesium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml, detect magnesium with atomic absorption spectrophotometer (AAS), average.Each content refers to table 1.
Embodiment 2
Change plant sample in embodiment 1 into masson pine skin, repeat embodiment 1 step.
Embodiment 3
Change plant sample in embodiment 1 into horse hair pine branch, repeat embodiment 1 step.
Embodiment 4
Change plant sample in embodiment 1 into red vertebra branch, repeat embodiment 1 step.
Embodiment 5
Get 600g plant sample Tokyo paulownia leaf be placed in baking oven keep temperature be 80 DEG C baking 8h, take out and pulverize, dry to constant weight at 85 DEG C again after crossing 40 mesh sieves, for subsequent use, get 100mg plant sample for subsequent use, put into the plastic centrifuge tube with a scale of 40ml, add the hot mixed in hydrochloric acid of 20ml 1mol/L of 80 DEG C, capping, with 200Hz hunting of frequency 60min, filter with quantitative filter paper, filter and terminate, extract filtrate 2ml, the lanthanum chloride 0.5ml of 5%, put into the volumetric flask of 25ml, be settled to 25ml with deionized water, shake up.Plant sample repeats 3 times as stated above, and the work not adding sample is blank, repeats 3 times with said method.Extract 20 μ g/ml potassium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the potassium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml.Detect potassium with atomic absorption spectrophotometer (AAS), average.Extract 100 μ g/ml calcium mark liquid 0,0.5,1,2,4ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the standard calcium serial solution of 0,2,4,8,16 μ g/ml.Calcium content is detected with atomic absorption spectrophotometer (AAS).Extract 20 μ g/ml magnesium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, the blank 2ml of each extraction, 5% lanthanum chloride 0.5ml add, add deionized water again to scale, obtain the magnesium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml, detect magnesium with atomic absorption spectrophotometer (AAS), average.Each content refers to table 1.
Embodiment 6
Change plant sample in embodiment 5 into masson pine skin, repeat embodiment 5 step.
Embodiment 7
Change plant sample in embodiment 5 into horse hair pine branch, repeat embodiment 5 step.
Embodiment 8
Change plant sample in embodiment 5 into red vertebra branch, repeat embodiment 5 step.
Embodiment 9
Get 500g plant sample Tokyo paulownia leaf be placed in baking oven keep temperature be 70 DEG C baking 28h, take out and pulverize, dry to constant weight at 100 DEG C again after crossing 60 mesh sieves, for subsequent use, get 250mg plant sample for subsequent use, put into the plastic centrifuge tube with a scale of 70ml, add the hot mixed in hydrochloric acid of 60ml 1mol/L of 50 DEG C, capping, with 200Hz hunting of frequency 75min, filter with quantitative filter paper, filter and terminate, extract filtrate 2ml, the lanthanum chloride 0.5ml of 5%, put into the volumetric flask of 25ml, be settled to 25ml with deionized water, shake up.Plant sample repeats 3 times as stated above, and the work not adding sample is blank, repeats 3 times with said method.Extract 20 μ g/ml potassium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the potassium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml.Detect potassium with atomic absorption spectrophotometer (AAS), average.Extract 100 μ g/ml calcium mark liquid 0,0.5,1,2,4ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the standard calcium serial solution of 0,2,4,8,16 μ g/ml.Calcium content is detected with atomic absorption spectrophotometer (AAS).Extract 20 μ g/ml magnesium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, the blank 2ml of each extraction, 5% lanthanum chloride 0.5ml add, add deionized water again to scale, obtain the magnesium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml, detect magnesium with atomic absorption spectrophotometer (AAS), average.Each content refers to table 1.
Embodiment 10
Change plant sample in embodiment 9 into masson pine skin, repeat embodiment 9 step.
Embodiment 11
Change plant sample in embodiment 9 into horse hair pine branch, repeat embodiment 9 step.
Embodiment 12
Change plant sample in embodiment 9 into red vertebra branch, repeat embodiment 9 step.
Embodiment 13
Get 500g plant sample Tokyo paulownia leaf be placed in baking oven keep temperature be 80 DEG C baking 30h, take out and pulverize, dry to constant weight at 65 DEG C again after crossing 36 mesh sieves, for subsequent use, get 200mg plant sample for subsequent use, put into the plastic centrifuge tube with a scale of 60ml, add the hot mixed in hydrochloric acid of the 50ml1mol/L of 100 DEG C, capping, with 200Hz hunting of frequency 80min, filter with quantitative filter paper, get filtrate, filter and terminate, extract filtrate 2ml, the lanthanum chloride 0.5ml of 5%, puts into the volumetric flask of 25ml, be settled to 25ml with deionized water, shake up.Plant sample repeats 3 times as stated above, and the work not adding sample is blank, repeats 3 times with said method.Extract 20 μ g/ml potassium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the potassium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml.Detect potassium with atomic absorption spectrophotometer (AAS), average.Extract 100 μ g/ml calcium mark liquid 0,0.5,1,2,4ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the standard calcium serial solution of 0,2,4,8,16 μ g/ml.Calcium content is detected with atomic absorption spectrophotometer (AAS).Extract 20 μ g/ml magnesium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, the blank 2ml of each extraction, 5% lanthanum chloride 0.5ml add, add deionized water again to scale, obtain the magnesium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml, detect magnesium with atomic absorption spectrophotometer (AAS), average.Each content refers to table 1.
Embodiment 14
Get 500g plant sample Tokyo paulownia leaf be placed in baking oven keep temperature be 60 DEG C baking 48h, take out and pulverize, dry to constant weight at 75 DEG C again after crossing 45 mesh sieves, for subsequent use, get 400mg plant sample for subsequent use, put into the plastic centrifuge tube with a scale of 90ml, add the hot mixed in hydrochloric acid of the 80ml1mol/L of 70 DEG C, capping, with 200Hz hunting of frequency 90min, filter with quantitative filter paper, filter and terminate, extract filtrate 2ml, the lanthanum chloride 0.5ml of 5%, put into the volumetric flask of 25ml, be settled to 25ml with deionized water, shake up.Plant sample repeats 3 times as stated above, and the work not adding sample is blank, repeats 3 times with said method.Extract 20 μ g/ml potassium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the potassium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml.Detect potassium with atomic absorption spectrophotometer (AAS), average.Extract 100 μ g/ml calcium mark liquid 0,0.5,1,2,4ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the standard calcium serial solution of 0,2,4,8,16 μ g/ml.Calcium content is detected with atomic absorption spectrophotometer (AAS).Extract 20 μ g/ml magnesium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, the blank 2ml of each extraction, 5% lanthanum chloride 0.5ml add, add deionized water again to scale, obtain the magnesium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml, detect magnesium with atomic absorption spectrophotometer (AAS), average.Each content refers to table 1.
Comparative example 1
Get 500g plant sample Tokyo paulownia leaf be placed in baking oven keep temperature be 60 DEG C baking 48h, take out and pulverize, dry to constant weight at 65 DEG C again after crossing 40 mesh sieves, for subsequent use, get 250mg plant sample for subsequent use, put into the plastic centrifuge tube with a scale of 150ml, add the hot mixed in hydrochloric acid of 50ml 1mol/L of 20 DEG C, capping, with 200Hz hunting of frequency 120min, filter with quantitative filter paper, get filtrate, filter and terminate, extract filtrate 2ml, the lanthanum chloride 0.5ml of 5%, puts into the volumetric flask of 25ml, be settled to 25ml with deionized water, shake up.Plant sample repeats 3 times as stated above, and the work not adding sample is blank, repeats 3 times with said method.Extract 20 μ g/ml potassium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5m add, then add deionized water to scale, obtain the potassium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml.Detect potassium with atomic absorption spectrophotometer (AAS), average.Extract 100 μ g/ml calcium mark liquid 0,0.5,1,2,4ml adds in 25ml volumetric flask respectively, each extract blank 2ml, 5% lanthanum chloride 0.5ml add, then add deionized water to scale, obtain the standard calcium serial solution of 0,2,4,8,16 μ g/ml.Calcium content is detected with atomic absorption spectrophotometer (AAS).Extract 20 μ g/ml magnesium mark liquid 0,0.5,1,2,3ml adds in 25ml volumetric flask respectively, the blank 2ml of each extraction, 5% lanthanum chloride 0.5ml add, add deionized water again to scale, obtain the magnesium standard serial solution of 0,0.4,0.8,1.6,2.4 μ g/ml, detect magnesium with atomic absorption spectrophotometer (AAS), average.Each content refers to table 1.
Comparative example 2
Change plant sample in comparative example 1 into masson pine skin, repeat comparative example 1 step, data are in table 1.
Comparative example 3
Change plant sample in comparative example 1 into horse hair pine branch, repeat comparative example 1 step, data are in table 1.
Comparative example 4
Change plant sample in comparative example 1 into red vertebra branch, repeat comparative example 1 step, data are in table 1.
Comparative example 5
The plant sample Tokyo paulownia leaf 250mg taking 18 mesh sieves puts into 30ml porcelain crucible, and 95% ethanolic solution first adding 1-2ml soaks sample.A small amount of deionized water soaks sample.Be placed on by crucible on electric furnace, crucible cover is tiltedly put, and regulates furnace temperature, slowly heating charing sample, avoids sample naked light burn and cause particulate ejection.Only could increase temperature after not smoldering, until sample is canescence, put into muffle furnace ashing process.In-furnace temperature remains on about 525 DEG C, ashing 1-2 hour, burns to ash content near-white.As carbon granule visible in sample, the melting parcel carbon granule surfaces such as the silicate of sodium, potassium or phosphate are described, make it isolated with oxygen, affect the complete ashing of sample.Meet this situation, several pure water can be added after the cooling period, dissolving salt film, make above carbon granule floats over, then to use water bath method, be reentered into calcination in muffle furnace fire.After abundant ashing, cooling, and with a small amount of water-wet ash content, gradation drips a small amount of 1.2mol/L dissolve with hydrochloric acid solution calcination, and during operation, careful anti-gray divides spatter loss.Question response adds 1.2mol/L10ml hydrochloric acid solution, is heated to boil, residue is dissolved after relaxing.Filter while hot, and with hot water wash crucible and residue for several times, filtrate is put in 50ml volumetric flask, and cooling constant volume obtains liquid to be measured.Plant sample repeats 3 times as stated above, and the blank not adding sample repeats 3 times as stated above.Potassium, content of calcium and magnesium method is measured with embodiment 1 (Bao Shidan, Soil Analysis in Agricultural Chemistry [M] Beijing: Chinese agriculture publishing house 2000) with the flame absorption process of atomic absorption spectrophotometer (AAS).Sample need be avoided to spatter in above-mentioned sample charing and calcination course of dissolution lose or dissolve not exclusively, thus cause element loss, testing result is on the low side.
Comparative example 6
Change plant sample in comparative example 5 into masson pine skin, repeat comparative example 5 step, data are in table 1.
Comparative example 7
Change plant sample in comparative example 5 into horse hair pine branch, repeat comparative example 5 step, data are in table 1.
Comparative example 8
Change plant sample in comparative example 5 into red vertebra branch, repeat comparative example 5 step, data are in table 1.
Testing result computing formula of the present invention:
Potassium of plants content (g/kg)=C*V*V1/V2/m/1000;
Calcium in Plants content (g/kg)=C*V*V1/V2/m/1000;
Plant content of magnesium (g/kg)=C*V*V1/V2/m/1000;
Coefficient of variation CV=SD/ mean value * 100.
Wherein, C: the potassium of mensuration, calcium, magnesium density (μ g/ml); V: survey and read liquid dilution volume (ml); V1: leaching liquor or salt acid eluate volume (ml); V2: extract testing liquid long-pending (ml); M: take plant sample quality (g); SD: the relative standard deviation of potassium, content of calcium and magnesium.
Testing result:
Table 1:
Note: alphabetical identical indicate without significant difference in the ranks, there were significant differences for the not identical expression of letter.
In table 1, " 20 DEG C of shaken at room temperature 120min " this row the data obtained is comparative example's 1 ~ 4 pair of potassium, content of calcium and magnesium detection gained; The data of " add 50 DEG C hydrochloric acid vibration 75min " this row gained are embodiment 9 ~ 12 pairs of potassium, content of calcium and magnesium detects gained; This row the data obtained is embodiment 1 ~ 4 pair of potassium, content of calcium and magnesium detects gained " to add 60 DEG C of hydrochloric acid vibration 60min "; This row the data obtained is embodiment 5 ~ 8 pairs of potassium, content of calcium and magnesium detects gained " to add 80 DEG C of hydrochloric acid vibration 60min "; " ashing method " this row the data obtained is comparative example's 5 ~ 8 pairs of potassium, content of calcium and magnesium detects gained.
As seen from Table 1, the inventive method detects the content there was no significant difference of the potassium of plant sample, content of calcium and magnesium and ashing method, but adds the method potassium of 20 DEG C of hydrochloric acid vibrations, content of calcium and magnesium and ashing method and have significant difference.The CV of the potassium of the inventive method, calcium, magnesium elements is all less than 10%, close with ashing method.Add the method for 20 DEG C of hydrochloric acid vibration survey calcium, the CV of magnesium elements is less than 10%, but the CV of potassium element has and is greater than 10%.As can be seen here, the precision of the inventive method mensuration potassium, calcium, magnesium elements is suitable with ashing method, and precision surveys potassium element higher than the method adding 20 DEG C of hydrochloric acid vibrations.
Recovery of standard addition detects
In order to check precision and the accuracy of the inventive method, weigh red each six parts of vertebra branch sample 250mg, wherein three parts add 100 μ g/ml potassium mark liquid 1ml, 100 μ g/ml magnesium mark liquid 2ml, 1000 μ g/ml calcium mark liquid 2ml respectively, add 1mol/L hydrochloric acid 20ml, in the process of the present invention oscillation treatment and detection potassium, content of calcium and magnesium.Remaining three parts add 100 μ g/ml potassium mark liquid 2ml, 100 μ g/ml magnesium mark liquid 1ml, 1000 μ g/ml calcium mark liquid 1ml respectively, add 1mol/L hydrochloric acid 21ml, oscillation treatment detect potassium, content of calcium and magnesium in the process of the present invention, calculates recovery of standard addition, draws data in table 2.
Wherein, recovery of standard addition=(detected value after mark-on-sample detection content/add scalar) × 100.
Table 2
From data in table 2, the inventive method recovery is that 95.02%-104.77, RSD are less than 7%; The method recovery adding 20 DEG C of hydrochloric acid vibrations is greater than 10% at 85.67%-89.23%, RSD; The ashing method recovery is that 94.52%-95.10%, RSD are less than 7%.It can thus be appreciated that the accuracy of the detection method of detection method and ashing method and precision are all higher, hydrochloric acid not the accuracy of heating means and precision on the low side.
Can find out that the sample ashing handling procedure of ashing method is loaded down with trivial details compared with inventive samples processing method program complexity by comparative example 5, there is hidden danger many in more difficult operation.Denseer white cigarette is emitted, contaminated environment when plant sample slowly carbonizes.Sample charing and calcination course of dissolution easily lose because careless manipulation causes sample splash to lose or dissolve hydrorrhea, cause element loss, affect testing result on the low side.Sample charing, high temperature ashing and calcination dissolves all needs careful operation in a heated condition, and labour intensity is high, and working pressure is large.Whole sample preparation duration, processes 20 samples and about uses 5 hours, and wherein sample charing and calcination dissolution filter and constant volume process then need to use 3 hours, length consuming time, complex operation, and personnel's fatigue, easily occur human error, detection efficiency is low.Therefore ashing method is not suitable for batch sample.The method adding 20 DEG C of hydrochloric acid vibrations is easy to operate, but potassium element lixiviate is insufficient, and the coefficient of variation of measurement result is higher, precision and poor accuracy.The inventive method once heats hydrochloric acid with 2000ml triangular flask, and to 50 DEG C-100 DEG C (preferably 50 ~ 60 DEG C), (there is thermal loss in adition process, add rear timely capping), more than 60 sample can be met use, only use general vibrating machine, the duration of oscillation is monitored at any time without the need to testing staff, 2 hours lixiviate process used times, efficiency is apparently higher than ashing method, personnel labor intensity obviously reduces, and potassium, calcium, magnesium lixiviate fully, are more suitable for batch sample and detect.
Plant sample grain size has certain influence for HCl extract.Sample particle is larger, is more difficult to infiltrate lixiviate abundant.Under normal circumstances, plant granule pulverization process crosses 18-60 mesh sieve.Normal temperature HCl extract tissue tight or cross 60 mesh sieves containing the high plant sample of lipid, even long-time vibration is also difficult to the potassium in vegetable cell, calcium, magnesium elements lixiviate abundant.As after the sieve process that comparatively 60 mesh sieve apertures (aperture 0.25mm) are less, plant granule is more tiny, just likely with potassium, calcium, magnesium elements in the abundant lixiviate plant of normal temperature hydrochloric acid.But the work that plant sample particle processes further detects for batch sample, increase operation easier and workload, waste time and energy.The inventive method is with masson pine, red vertebra, Tokyo Tong Deng tissue tight or cross 40 mesh sieve process containing the skin of the high difficult infiltration of plants sample of lipid, branch, foliage organ, potassium, calcium, magnesium determination result precision and accuracy are high, this illustrates that detection method is applicable to multiclass plant sample, sample particle granularity is within routine practice, without particular/special requirement, the sample preparation of the inventive method is simple.
The inventive method is simple and easy, and convenient operation controls, and accurately and reliably, detection efficiency is high for testing result, and instrument facility is simple, is easily equipped with.Be not only applicable to polymorphic type plant sample potassium, content of calcium and magnesium detects, and a certain amount of hydrochloric acid is once heated to 50 ~ 100 DEG C (preferably 50 ~ 60 DEG C), temperature range is easy to control, and the sample of single treatment is many, and efficiency is high.Human users is convenient, and working load is low, is applicable to batch sample and detects, for the work such as nutrition diagnosis, plant research provides believable data.
The aforementioned description to concrete exemplary of the present invention is to illustrate and the object of illustration.These descriptions not want the present invention to be defined as disclosed precise forms, and obviously, according to above-mentioned instruction, can much change and change.The object selected exemplary embodiment and describe is to explain certain principles of the present invention and practical application thereof, thus those skilled in the art can be realized and utilize various different exemplary of the present invention and various different selection and change.Scope of the present invention is intended to limited by claims and equivalents thereof.
Claims (9)
1. detect a method for potassium in plant, content of calcium and magnesium, it is characterized in that, comprise following operation: pretreated plant sample 65 ~ 100 DEG C is dried to constant weight, the vibration of heating mixed in hydrochloric acid, filters, gets filtrate, the content of potassium, calcium, magnesium is measured after dilution constant volume.
2. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: described hot hydrochloric acid refers to that temperature is the hydrochloric acid of 50 ~ 100 DEG C.
3. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: described hot hydrochloric acid refers to that temperature is the hydrochloric acid of 50 ~ 60 DEG C.
4. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: described hot hydrochloric acid volumetric concentration is 1mol/L.
5. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: described 65 ~ 100 DEG C of plant samples of drying to constant weight, add the hot hydrochloric acid of 20 ~ 100ml according to the amount of every 100 ~ 400mg.
6. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: described pre-service, for plant sample is toasted 8 ~ 48h through 60 ~ 80 DEG C, is pulverized and crosses 18 ~ 60 mesh sieves.
7. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: described pre-service, for plant sample is toasted 8 ~ 48h through 60 ~ 80 DEG C, is pulverized and crosses 40 ~ 60 mesh sieves.
8. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: described heating mixed in hydrochloric acid vibration 60 ~ 90min, oscillation frequency is 200Hz.
9. detect the method for potassium, content of calcium and magnesium in plant according to claim 1, it is characterized in that: dry the plant sample to constant weight, put into the plastic centrifuge tube with a scale of 40 ~ 100ml, heating mixed in hydrochloric acid.
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| CN110813206A (en) * | 2019-10-16 | 2020-02-21 | 广西大学 | Method for removing potassium ions, calcium ions and magnesium ions in fast-growing eucalyptus |
| CN114184441A (en) * | 2021-10-19 | 2022-03-15 | 威凯检测技术有限公司 | Preparation device and method of animal-derived medical instrument biological safety evaluation experiment leaching liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110813206A (en) * | 2019-10-16 | 2020-02-21 | 广西大学 | Method for removing potassium ions, calcium ions and magnesium ions in fast-growing eucalyptus |
| CN110672537A (en) * | 2019-11-12 | 2020-01-10 | 金花企业(集团)股份有限公司西安金花制药厂 | Method for determining potassium, sodium, magnesium, iron and zinc in artificial tiger bone powder |
| CN114184441A (en) * | 2021-10-19 | 2022-03-15 | 威凯检测技术有限公司 | Preparation device and method of animal-derived medical instrument biological safety evaluation experiment leaching liquor |
| CN114184441B (en) * | 2021-10-19 | 2024-04-05 | 威凯检测技术有限公司 | Preparation device and method of animal-derived medical instrument biosafety evaluation experiment leaching solution |
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Application publication date: 20150923 |