CN103969397A - Method for detecting organic carbon in plants and soil and heating device thereof - Google Patents
Method for detecting organic carbon in plants and soil and heating device thereof Download PDFInfo
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- CN103969397A CN103969397A CN201410205219.5A CN201410205219A CN103969397A CN 103969397 A CN103969397 A CN 103969397A CN 201410205219 A CN201410205219 A CN 201410205219A CN 103969397 A CN103969397 A CN 103969397A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 55
- 238000010438 heat treatment Methods 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000002689 soil Substances 0.000 title abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 69
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000001514 detection method Methods 0.000 claims abstract description 32
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 64
- 125000006850 spacer group Chemical group 0.000 claims description 47
- 229910052742 iron Inorganic materials 0.000 claims description 32
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 31
- 238000004448 titration Methods 0.000 claims description 24
- 238000007254 oxidation reaction Methods 0.000 claims description 17
- 239000004016 soil organic matter Substances 0.000 claims description 16
- 239000012535 impurity Substances 0.000 claims description 5
- 235000003891 ferrous sulphate Nutrition 0.000 abstract description 9
- 239000011790 ferrous sulphate Substances 0.000 abstract description 9
- 230000001590 oxidative effect Effects 0.000 abstract 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 59
- 241000196324 Embryophyta Species 0.000 description 39
- 239000007788 liquid Substances 0.000 description 10
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 238000009835 boiling Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000011229 interlayer Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 239000012925 reference material Substances 0.000 description 6
- 238000004364 calculation method Methods 0.000 description 4
- 230000029087 digestion Effects 0.000 description 4
- 239000012496 blank sample Substances 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 239000002274 desiccant Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- UPLPHRJJTCUQAY-WIRWPRASSA-N 2,3-thioepoxy madol Chemical compound C([C@@H]1CC2)[C@@H]3S[C@@H]3C[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@](C)(O)[C@@]2(C)CC1 UPLPHRJJTCUQAY-WIRWPRASSA-N 0.000 description 1
- 244000050510 Cunninghamia lanceolata Species 0.000 description 1
- 101100489867 Mus musculus Got2 gene Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
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- 230000006641 stabilisation Effects 0.000 description 1
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- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a detection method and in particular relates to a method for detecting organic carbon in plants and soil and a heating device of the method. The method for detecting organic carbon in plants and soil comprises the following steps: pretreating a plant sample or a soil sample, mixing the pretreated plant sample or the pretreated soil sample, potassium dichromate solution and concentrated sulfuric acid solution in a triangular flask, heating to carry out oxidizing reaction, adding distilled water after the reaction is ended, cooling and adding phenanthroline solution as an indicator, titrating the residual potassium dichromate in the oxidizing reaction by using ferrous sulfate solution, and calculating the content of organic carbon, wherein the oxidizing reaction refers to reaction under the condition of normal pressure steam generated by water at the temperature of 90-100 DEG C for 20-60 minutes. The normal pressure steam heating method is simple to operate and easy to control, the temperature in a water bath kettle is stable and easy to control, the sample is uniformly heated and fully digested, and the method is safe, environmentally friendly, high in detection reproducibility, accurate and efficient.
Description
Technical field
The present invention relates to a kind of detection method, relate in particular to a Plants, soil organic matter detection method and heating arrangement thereof.
Background technology
Global Carbon converges in research, plant, Organic Carbon of Forest Soils content are the key indexs of evaluating the solid carbon ability of the ecosystem, and in prior art, main potassium dichromate oxidation-Outside Heating Method, Boiling bath method, electric hot plate heating, the graphite furnace methods such as cooking method that disappear that adopt are carried out organic carbon detection.
Described in GB GB7857-87, forestry industry standard LY/T1237-1999, potassium dichromate oxidation-Outside Heating Method is with adjustable electric cooking stove to plant or pedotheque, potassium bichromate solution, the heating of sulfuric acid solution three mixed liquor, and glycerine or vegetable oil are heating medium.Disappear and boil 170-180 ℃ of oil bath of pipe immersion, wait to manage interior solution and keep boiling to take out for 5 minutes.Organic carbon in plant or soil is oxidized in the above conditions, and remaining potassium bichromate solution carrys out titration with copperas solution, can calculate the content of organic carbon from consumed copperas solution amount.There is following problem in said method: high temperature oils is inflammable and explosive, dangerous hidden danger; Disappear and boil temperature and be difficult for stablely, disappear and boil liquid fluidized state and Digestion time is difficult to grasp in different pipes, temperature just changes and Digestion time length all can affect organic carbon oxidation reaction, causes testing result inaccurate; Utensil and environmental pollution are serious, and vessel greasy dirt is difficult to be cleaned, time-consuming; It is healthy that environmental pollution has a strong impact on testing staff.
Need triangular flask is under water during boiling water bath heating, it is improper that water level is controlled, triangular flask is affected by buoyancy of water can be when placing or topple over during boiling water heating and cause in bottle in potassium bichromate solution and sulfuric acid solution inflow boiling water, this not only causes the sample that boils failure of disappearing again to weigh and disappear and boils, and the strong acid solution flowing out will, to generation severe oxidation corrosion such as pot body and heating tubes, cause the potential safety hazards such as pot body seepage or circuit damage.
Have in document and to propose to disappear and boil instrument and disappear and boil with electric hot plate or graphite furnace etc., list of references is as (two kinds of heating and decompose methods are measured the comparative analysis [J] of the soil organism, Wang Yucan, Zhu Jianping, Sun Huichan, Guangdong Forestry science, 2009 (4)); List of references is as (different digestion procedures are measured soil organic matter content [J], Shao Ming, Liaoning agricultural occupation technical college journal, 2009,11 (1)).Above-mentioned instrument possesses heating, temperature adjustment and temperature incubation function, disappear and boil Guan Fangzhi instrument heating position and disappear and boil, although temperature is controlled, avoided pollution, eliminate potential safety hazard, but still existed the disappearing of diverse location at heating position to boil liquid fluidized state and the difficult problem of holding of Digestion time.While said method need boil by disappearing liquid and wash in triangular flask so that titration increases operation virtually.
Above-mentioned boiling water bath, electric hot plate or graphite furnace etc. disappear and boil instrument type of heating and need determine separately correction coefficient.List of references is as (in potassium bichromate titrimetric method, different heating mode is measured the comparative studies of the soil organism, Ji Tianwei, Zhejiang Agriculture journal, 2005,17 (5)); List of references is as (comparison that volumetric determination soil organism difference is cleared up mode, Lang Songyan, Zhang Fujin, Li Xiuping etc., Inner Mongol agricultural science and technology 2009 (1)).
Plant or soil organic matter can also detect by TOC analyser, and it is by carbon complete oxidation in sample, generate CO
2, non-dispersive formula infrared analyzer (NDIR) spectrum quantitative measurment total carbon and total inorganic carbon (TIC) value, by total carbon and total inorganic carbon (TIC) IC the difference relation that equals Organic Carbon TOC draw its content.Although TOC analyser accuracy rate is higher, the instrument switch machine used time is longer, and the detection time of every workday is limited, generally only can detect the sample of 20 left and right, is not suitable for batch sample and detects.
Summary of the invention
The present invention measures a kind of detection method accurately and efficiently and heating arrangement thereof is provided for agriculture and forestry plant, soil organic carbon.Overcome current organic carbon detection method and existed potential safety hazard serious, the problem such as heating is uneven, and temperature is wayward.
Object of the present invention is achieved through the following technical solutions:
One Plants, soil organic matter detection method, the method is that plant sample or pedotheque are carried out to pre-service, by the pre-service plant sample of pre-service gained or pre-service pedotheque, potassium bichromate solution, concentrated sulfuric acid solution three is placed in triangular flask and mixes, oxidation reaction is carried out in heating, after finishing, reaction adds distilled water, cooling rear interpolation Phen solution is as indicator, then use the remaining potassium dichromate of copperas solution titration oxidation reaction, calculate organic carbon content, described oxidation reaction is to react 20～60 minutes under the atmospheric steam condition producing at 90～100 ℃ of water.
Preferably: described oxidation reaction is to react 30 minutes under the atmospheric steam condition producing at 96～100 ℃ of water.
Preferably: described plant sample was through 60～80 ℃ of bakings 8～48 hours, pulverized 0.25mm sieve, through 65～100 ℃, dry to constant weight and make pre-service plant sample, every 20mg～35mg pre-service plant sample need add 8ml～15mL potassium bichromate solution and 8ml～15mL concentrated sulfuric acid solution, and the potassium bichromate solution wherein adding and concentrated sulfuric acid solution volume ratio are 1:1.
Preferably: described pedotheque through air-dry removal of impurities, ground 2mm sieve, by inquartation, get 2/4 sample of crossing after 2mm sieve, grind again 0.25mm sieve series and obtained pre-service pedotheque, every 100～800mg pre-service pedotheque need add 5ml～10mL potassium bichromate solution solution and 5ml～10mL concentrated sulfuric acid solution, and the potassium bichromate solution wherein adding and concentrated sulfuric acid solution volume ratio are 1:1.
Preferably: described potassium bichromate solution concentration is 0.6mol/L～1.0mol/L, wherein potassium bichromate solution optimum concentration is 0.8mol/L; Described concentrated sulfuric acid solution massfraction is 98%.
Preferably: described pre-service plant sample, concentrated sulfuric acid solution, potassium bichromate solution three be remaining 0.1mol/L～0.6mol/L copperas solution titration for potassium bichromate solution after oxidation reaction, and wherein copperas solution optimum concentration is 0.4mol/L; Described pre-service pedotheque, concentrated sulfuric acid solution, potassium bichromate solution three be remaining 0.1mol/L～0.6mol/L copperas solution titration for potassium bichromate solution after oxidation reaction, and wherein copperas solution optimum concentration is 0.2mol/L.
The heating arrangement that described plant, soil organic matter detection method are used, described heating arrangement is comprised of thermostat water bath, spacer for hanger and capping, described thermostat water bath comprises tank, tank is provided with capping and seals, described capping top is provided with handle, it is characterized in that: on described spacer for hanger, have some eyelets, spacer for hanger is horizontally set in tank, described spacer for hanger has 1/2nd to 2/3rds tank height apart from bottom of gullet, and spacer for hanger is higher than water level in tank.
Preferably: described capping is that the degree of depth is the iron square groove of 4～6 centimetres, and four edges of described iron square groove notch are equipped with rubber strip, and the notch edge of iron square groove presses on the notch edge of tank.
Beneficial effect of the present invention:
(1) the present invention is on the basis of water-bath, in water-bath tank, arrange one higher than the spacer for hanger of tank water level, the triangular flask that reactant liquor is housed is placed on spacer for hanger, the steam that water-bath is produced heats the reactant liquor in triangular flask, four edges of iron square groove notch install rubber strip additional, iron square groove is contacted with water-bath closely, reduce vapour losses.The spacer for hanger of placing triangular flask exceeds water level, and triangular flask is under water, has avoided the unstable initiation of sample placement to disappear and has boiled the problem of failure, has prevented heating instrument to be subject to the hidden danger of havoc.The easy control simple to operate of atmospheric steam heating, the temperature stabilization in water-bath is easily controlled, and sample is heated evenly, and disappears and boils fully, and the present invention is safety and environmental protection not only, and it is good to detect repeatability, precise and high efficiency.
(2) oxidation reaction and titration all can be carried out in triangular flask, and without shifting link, operation is simplified, zero loss.
(3) the present invention can carry out batch sample detection, as to take the water-bath of octal size be heating arrangement basis, arranges after interlayer and capping, once can the sample of 40 150ml triangular flask splendid attires be disappeared and be boiled, and work efficiency is high.
(4) testing result of the present invention directly adopts the computing formula of GB organic carbon:
Plant organic carbon content (g/kg)=0.8*V
1* (V
0-V
2)/V
0* 0.003*1.1/m*1000
Soil organic carbon (g/kg)=0.8*V
1* (V
0-V
2)/V
0* 0.003*1.1/ (m*k) * 1000
V
1: the volume (ml) that adds potassium dichromate
V
0: blank sample consumes ferrous sulphate volume (ml)
V
2: sample consumes ferrous sulphate volume (ml)
M: sample quality (g)
K: pedotheque Water coefficient
The present invention is without determining in addition correction coefficient, and error is little, detects accurately.
(5) plant of the present invention, soil organic carbon detection precision and accuracy are high.Organic carbon testing result of the present invention contrasts there was no significant difference with TOC analyser testing result.
Accompanying drawing explanation
Fig. 1 is heating arrangement structural representation of the present invention;
Description of reference numerals:
1, thermostat water bath 2, capping 3, spacer for hanger 4, tank 5, handle.
Embodiment
Below in conjunction with specific embodiment, the present invention is done to further detailed elaboration, but embodiments of the present invention are not limited to the scope that embodiment represents.These embodiment are only for the present invention is described, but not for limiting the scope of the invention.In addition, after reading content of the present invention, those skilled in the art can do various modifications to the present invention, and these equivalent variations fall within appended claims limited range of the present invention equally.
Embodiment 1
The heating arrangement that this plant organic carbon detection method is used, by thermostat water bath 1, capping 2, spacer for hanger 3, formed, the interior spacer for hanger 3 that is laterally equipped with of tank 4 of described thermostat water bath 1 (water-bath is biserial octal electric-heated thermostatic water bath (HWS-28)), 10 perforates are set on spacer for hanger 3, regulate the position of spacer for hanger 3 to tank 1/4th two height, control height of water level, make it lower than spacer for hanger 3 height.At the triangular flask bottleneck that adds each reactive material, load onto a curved neck funnel, then on tank, cover capping 2, described capping 2 is that the degree of depth is the iron square groove of 4 centimetres, capping 2 tops are also provided with handle 5, iron square groove notch edge presses on tank 4 notch edges tank 4 is sealed, described four edges of iron square groove notch add rubber strip, and iron square groove is contacted with tank 4 closely, reduce vapour losses.
10g plant leaf blade sample is placed in to 60 ℃ of baking boxs baking 48 hours, after taking-up, pulverizes, under 65 ℃ of conditions, dry to constant weight and make pre-service plant sample after crossing 0.25mm sieve, be positioned over that in the exsiccator of drying agent, to be cooled to room temperature standby.Get pre-service plant sample 20mg and be placed in 150ml triangular flask, add 0.6mol/l potassium bichromate solution 8ml, massfraction is 98% concentrated sulfuric acid solution (density is 1.84g/mL) 8ml, after shaking up, triangular flask is put on water-bath interlayer, covered and enclosed, normal press control bath temperature is 90 ℃, after the steam heating 60min that utilizes water-bath to produce, take out, adding 16ml distilled water shakes up and is cooled to room temperature, adding 3 phenanthroline solution (concentration is 1.485g/100mL) shakes up, with the titration of 0.1mol/l copperas solution, disappear and boil liquid, when solution colour by orange become bluish-green, from bluish-green becoming, stopping titration when reddish brown, not add the work blank of sample, with the method, repeat blank 2 times.Record respectively copperas solution consumption and calculate organic carbon content.
Embodiment 2
The heating arrangement that this plant organic carbon detection method is used, by thermostat water bath 1, capping 2, spacer for hanger 3, formed, the interior spacer for hanger 3 that is laterally equipped with of tank 4 of described thermostat water bath 1 (water-bath is biserial octal electric-heated thermostatic water bath (HWS-28)), 15 perforates are set on spacer for hanger 3, regulate the position of spacer for hanger 3 to tank 7/40ths two height, control height of water level, make it lower than spacer for hanger 3 height.At the triangular flask bottleneck that adds each reactive material, load onto a curved neck funnel, then on tank 4, cover capping 2, described capping 2 is that the degree of depth is the iron square groove of 5 centimetres, capping 2 tops are also provided with handle 5, iron square groove notch edge presses on tank 4 notch edges tank 4 is sealed, described four edges of iron square groove notch add rubber strip, and iron square groove is contacted with tank 4 closely, reduce vapour losses.
10g plant leaf blade sample is placed in to 70 ℃ of baking boxs baking 20 hours, after taking-up, pulverizes, under 80 ℃ of conditions, dry to constant weight and make pre-service plant sample after crossing 0.25mm sieve, be positioned over that in the exsiccator of drying agent, to be cooled to room temperature standby.Get pre-service plant sample 30mg and be placed in 150ml triangular flask, add 0.8mol/l potassium bichromate solution 10ml, massfraction is 98% concentrated sulfuric acid solution 10ml, after shaking up, triangular flask is put on water-bath interlayer, covered and enclosed, normal press control temperature is 96 ℃, after the steam heating 30min that utilizes water-bath to produce, take out, adding 20ml distilled water shakes up and is cooled to room temperature, adding 5 phenanthroline solution (concentration is 1.485g/100mL) shakes up, with the titration of 0.4mol/l copperas solution, disappear and boil liquid, when solution colour by orange become bluish-green, from bluish-green becoming, stopping titration when reddish brown, not add the work blank of sample, with the method, repeat blank 2 times.Record respectively copperas solution consumption and calculate organic carbon content.
Embodiment 3
The heating arrangement that this plant organic carbon detection method is used, by thermostat water bath 1, capping 2, spacer for hanger 3, formed, the interior spacer for hanger 3 that is laterally equipped with of tank 4 of described thermostat water bath 1 (water-bath is biserial octal electric-heated thermostatic water bath (HWS-28)), 20 perforates are set on spacer for hanger 3, regulate the position of spacer for hanger 3 to tank 2/4ths three height, control height of water level, make it lower than spacer for hanger 3 height.At the triangular flask bottleneck that adds each reactive material, load onto a curved neck funnel, then on tank 4, cover capping 2, described capping 2 is that the degree of depth is the iron square groove of 6 centimetres, capping 2 tops are also provided with handle 5, iron square groove notch edge presses on tank 4 notch edges tank 4 is sealed, described four edges of iron square groove notch add rubber strip, and iron square groove is contacted with tank 4 closely, reduce vapour losses.
10g Plant litterfall matter sample is placed in to 80 ℃ of baking boxs baking 8 hours, after taking-up, pulverizes, under 100 ℃ of conditions, dry to constant weight and make pre-service plant sample after crossing 0.25mm sieve, be positioned over that in the exsiccator of drying agent, to be cooled to room temperature standby.Get pre-service plant sample 35mg and be placed in 150ml triangular flask, add 1.0mol/l potassium bichromate solution 15ml, massfraction is 98% concentrated sulfuric acid solution 15ml, after shaking up, triangular flask is put on water-bath spacer for hanger, covered and enclosed, normal press control bath temperature is 100 ℃, after the steam heating 20min that utilizes water-bath to produce, take out, adding 30ml distilled water shakes up and is cooled to room temperature, adding 6 phenanthroline solution (concentration is 1.485g/100mL) shakes up, with the titration of 0.6mol/l copperas solution, disappear and boil liquid, when solution colour by orange become bluish-green, from bluish-green becoming, stopping titration when reddish brown, not add the work blank of sample, with the method, repeat blank 2 times.Record respectively copperas solution consumption and calculate organic carbon content.
Embodiment 4
The heating arrangement that this soil organic matter detection method is used, by thermostat water bath 1, capping 2, spacer for hanger 3, formed, the interior spacer for hanger 3 that is laterally equipped with of tank 4 of described thermostat water bath 1 (water-bath is biserial octal electric-heated thermostatic water bath (HWS-28)), 15 perforates are set on spacer for hanger 3, regulate the position of spacer for hanger 3 to tank 1/4th two height, control height of water level, make it lower than spacer for hanger 3 height.At the triangular flask bottleneck that adds each reactive material, load onto a curved neck funnel, then on tank 4, cover capping 2, described capping 2 is that the degree of depth is the iron square groove of 4 centimetres, capping 2 tops are also provided with handle 5, iron square groove notch edge presses on tank 4 notch edges tank 4 is sealed, described four edges of iron square groove notch add rubber strip, and iron square groove is contacted with tank 4 closely, reduce vapour losses.
100g pedotheque is air-dry, removal of impurities, the rear 2mm sieve of crossing of grinding, get 2/4 sample of crossing after 2mm sieve by inquartation, then ground 0.25mm sieve series and obtain pre-service pedotheque.Get 100mg pre-service pedotheque, add 0.6mol/l potassium bichromate solution 5ml, massfraction is 98% concentrated sulfuric acid solution 5ml, after shaking up, triangular flask is put on water-bath spacer for hanger, covered and enclosed, normal press control bath temperature is 90 ℃, after the Steam Heating 60min that utilizes water-bath to produce, take out, adding 10ml distilled water shakes up and is cooled to room temperature, adding 2 phenanthroline solution (concentration is 1.485g/100mL) shakes up, with the titration of 0.1mol/l copperas solution, disappear and boil liquid, when solution colour becomes bluish-greenly by orange, from bluish-green becoming, stopping titration when reddish brown.Not add the work blank of sample, with the method, repeat blank 2 times.Record respectively copperas solution consumption and calculate organic carbon content.Separately get pedotheque 10g and dry to constant weight under 105 ℃ of conditions, be put in exsiccator cooling after, weigh immediately, with the Water coefficient of calculation sample.
Embodiment 5
The heating arrangement that this plant organic carbon detection method is used, by thermostat water bath 1, capping 2, spacer for hanger 3, formed, the interior spacer for hanger 3 that is laterally equipped with of tank 4 of described thermostat water bath 1 (water-bath is biserial octal electric-heated thermostatic water bath (HWS-28)), 17 perforates are set on spacer for hanger 3, regulate the position of spacer for hanger 3 to tank 7/40ths two height, control height of water level, make it lower than spacer for hanger 3 height.At the triangular flask bottleneck that adds each reactive material, load onto a curved neck funnel, then on tank 4, cover capping 2, described capping 2 is that the degree of depth is the iron square groove of 5 centimetres, capping 2 tops are also provided with handle 5, iron square groove notch edge presses on tank 4 notch edges tank 4 is sealed, described four edges of iron square groove notch add rubber strip, and iron square groove is contacted with tank 4 closely, reduce vapour losses.
100g pedotheque is air-dry, removal of impurities, the rear 2mm sieve of crossing of grinding, get 2/4 sample of crossing after 2mm sieve by inquartation, then ground 0.25mm sieve.Get 500mg pre-service pedotheque, add 0.8mol/l potassium bichromate solution 8ml, massfraction is 98% concentrated sulfuric acid solution 8ml, after shaking up, triangular flask is put on water-bath interlayer, covered and enclosed, normal press control bath temperature is 98 ℃, after the steam heating 30min that utilizes water-bath to produce, take out, adding 16ml distilled water shakes up and is cooled to room temperature, adding 5 phenanthroline solution (concentration is 1.485g/100mL) shakes up, with the titration of 0.2mol/l copperas solution, disappear and boil liquid, when solution colour by orange become bluish-green, from bluish-green, becoming that to stop titration when reddish brown blank not add the work of sample, with the method, repeat blank 2 times.Record respectively copperas solution consumption and calculate organic carbon content.Separately get pedotheque 10g and dry to constant weight under 105 ℃ of conditions, be put in exsiccator cooling after, weigh immediately, with the Water coefficient of calculation sample.
Embodiment 6
The heating arrangement that this plant organic carbon detection method is used, by thermostat water bath 1, capping 2, spacer for hanger 3, formed, the interior spacer for hanger 3 that is laterally equipped with of tank 4 of described thermostat water bath 1 (water-bath is biserial octal electric-heated thermostatic water bath (HWS-28)), 25 perforates are set on spacer for hanger 3, regulate the position of spacer for hanger 3 to tank 2/4ths three height, control height of water level, make it lower than spacer for hanger 3 height.At the triangular flask bottleneck that adds each reactive material, load onto a curved neck funnel, then on tank 4, cover capping 2, described capping 2 is that the degree of depth is the iron square groove of 6 centimetres, capping 2 tops are also provided with handle 5, iron square groove notch edge presses on tank 4 notch edges tank 4 is sealed, described four edges of iron square groove notch add rubber strip, and iron square groove is contacted with tank 4 closely, reduce vapour losses.
100g pedotheque is air-dry, removal of impurities, the rear 2mm sieve of crossing of grinding, get 2/4 sample of crossing after 2mm sieve by inquartation, then ground 0.25mm sieve.Get 800mg pre-service pedotheque, add 1.0mol/l potassium bichromate solution 10ml, massfraction is 98% concentrated sulfuric acid solution 10ml, after shaking up, triangular flask is put on water-bath interlayer, covered and enclosed, normal press control bath temperature is 100 ℃, after the steam heating 30min that utilizes water-bath to produce, take out, adding 20ml distilled water shakes up and is cooled to room temperature, adding 5 or 6 phenanthroline solution (concentration is 1.485g/100mL) shakes up, with the titration of 0.6mol/l copperas solution, disappear and boil liquid, when solution colour by orange become bluish-green, from bluish-green becoming, stopping titration when reddish brown.Not add the work blank of sample, with the method, repeat blank 2 times.Record respectively copperas solution consumption and calculate organic carbon content.Separately get pedotheque 10g and dry to constant weight under 105 ℃ of conditions, be put in exsiccator cooling after, weigh immediately, with the Water coefficient of calculation sample.
It is below contrast test.
One, material and equipment
1, plant sample (from erythrophloeum ferdii leaf and the fragrant China fir Litter-fall in the summer stone mountain artificial forest of Tropical Forest experimental center, Chinese forest-science academy)
2, pedotheque (from Tropical Forest experimental center, Chinese forest-science academy summer stone mountain)
3,0.8mol/L potassium bichromate solution
4, the concentrated sulfuric acid solution (density 1.84g/mL) that massfraction is 98%
5,1.485g/100mL phenanthroline solution
6,0.4mol/L copperas solution, 0.2mol/L copperas solution
7, Potassium Hydrogen Phthalate (top grade is pure)
8, electronic balance (ten thousand/precision)
9, electronic balance (one of percentage precision)
10, the heating arrangement identical with embodiment 2
11, TOC analyser (Shimadzu TOC-L SSM/5000A)
Two, method
According to different heating mode, be divided into atmospheric steam group, TOC analyser group.
Plant leaf blade and Litter-fall sample are pulverized after drying 24 hours immediately at 65 ℃, and crossed 0.25mm sieve, plant sample is dried to constant weight under 65 ℃ of conditions, be positioned over that in exsiccator, to be cooled to room temperature stand-by.
After pedotheque is air-dry, first ground 2mm sieve, and with inquartation, got 2/4 sample of crossing 2mm sieve and ground 0.25mm sieve, get 10g 105 ℃ dry to constant weight after, be put in exsiccator cooling after, weigh immediately, with the Water coefficient of calculation sample.Remaining sample is stand-by.
Potassium Hydrogen Phthalate is taken out at 110 ℃ to be placed in exsiccator cooling standby after drying 3 hours, for measuring blank recovery of standard addition.
Atmospheric steam group: get above-mentioned pretreated plant sample 30mg and be placed in 150mL triangular flask, the 0.8mol/L potassium bichromate solution that adds 10mL, 10mL massfraction is 98% concentrated sulfuric acid solution, after shaking up, triangular flask is put on water-bath spacer for hanger, normal press control bath temperature is 98 ℃, after the steam heating 30min that utilizes water-bath to produce, take out, adding 10mL distilled water shakes up and is cooled to room temperature, adding 6 Phen solution shakes up, with the titration of 0.4mol/L copperas solution, when solution colour by orange become bluish-green, from bluish-green becoming, stopping titration when reddish brown, record copperas solution consumption, be total to three parts of above-mentioned plant samples of parallel processing.Not add the work blank of sample, in kind repeat blank 2 times, try to achieve copperas solution consumption mean value and make blank value.Get Potassium Hydrogen Phthalate 30mg and replace sample by above method repetitive operation, repeat 3 times, record respectively the coefficient of variation (CV) that copperas solution consumption calculates organic carbon content, organic carbon content.
Get above-mentioned pretreated pedotheque 300mg and be placed in 150mL triangular flask, by above method operation detection.
TOC analyser group: get above-mentioned pretreated plant sample 30mg and be laid in the example boat of TOC analyser, put into respectively burning chamber, under 900 ℃ of conditions, measure total carbon, under 200 ℃ of conditions, survey inorganic carbon amount, thereby draw organic carbon amount, each sample repetitive operation is measured organic carbon content 3 times, and tries to achieve its coefficient of variation (CV).Get Potassium Hydrogen Phthalate 30mg and repeat 3 times by above method, measure organic carbon amount, calculate blank recovery of standard addition.
Get above-mentioned pretreated pedotheque 300mg and be laid in the example boat of TOC analyser, by above method operation detection.
Organic carbon determination result to atmospheric steam group and TOC analyser group is carried out variance analysis, detects and has there was no significant difference.
Atmospheric steam group computing formula is as follows:
1, plant organic carbon content (g/kg)=0.8*V
1* (V
0-V
2)/V
0* 0.003*1.1/m*1000
2, soil organic carbon (g/kg)=0.8*V
1* (V
0-V
2)/V
0* 0.003*1.1/ (m*k) * 1000
3, pedotheque Water coefficient k=(1-(10.00 – m
1)/m
1)) * 100%
V
1: the volume (ml) that adds potassium dichromate
V
0: blank sample consumes ferrous sulphate volume (ml)
V
2: sample consumes ferrous sulphate volume (ml)
M: dry sample quality (g)
K: pedotheque Water coefficient
M
1: 105 ℃ of weight that dry to constant weight of 10g wind desiceted soil (g)
4, the theoretical carbon content of blank recovery of standard addition %=Potassium Hydrogen Phthalate practical measurement carbon content (g/kg)/Potassium Hydrogen Phthalate (g/kg) * 100%
5, Potassium Hydrogen Phthalate practical measurement carbon content (g/kg)=0.8*V
potassium dichromate* (V
blank-V
reference material) * 0.003*1.1*100/ (V
blank* M
reference material) * 100%
The theoretical carbon content (g/kg)=470.1 (g/kg) of Potassium Hydrogen Phthalate
Wherein: V
potassium dichromaterefer to add potassium dichromate amount (ml), V
blankrefer to that blank sample consumes ferrous sulphate amount (ml), V
reference materialrefer to that reference material Potassium Hydrogen Phthalate consumes ferrous sulphate amount (ml), M
reference materialrefer to dry the weighing (g) of reference material Potassium Hydrogen Phthalate.
Three, result
Experimental result is in Table 1 and table 2.
Two kinds of method organic carbon testing result contrasts of table 1
Note: 1, two of plant sample blank volumes that consume ferrous sulphate are respectively 20.00ml, 20.05ml, and blank average is 20.025ml; Two blank volumes that consume ferrous sulphate of pedotheque are respectively 20ml, 20ml, and blank average is 20ml.2, the Water coefficient of air-dry pedotheque is 97.6%.3, identical the indicating without significant difference of letter between row, there were significant differences for the not identical expression of letter.
Two kinds of method recovery testing result contrasts of table 2
The inventive method and TOC analysis-e/or determining data Analysis of variance, organic carbon content is without significant difference, and the coefficient of variation of this experiment is all less than 3%, and precision is good.The inventive method recovery is 103.68%, between 95%-105%; The TOC analyser recovery is 99.72%, between 95%-105%.The accuracy of the detection method of the inventive method and TOC analyser is all higher.Because the TOC analyser switching on and shutting down used time is longer, the detection time of every workday is limited, generally only can detect the sample of 20 left and right, is not suitable for batch sample and detects.The inventive method every workday can disappear boils and detects 60-80 sample, and efficiency, apparently higher than TOC analyser, is more suitable for batch sample and detects.
The inventive method is placed directly in triangular flask on the interlayer of water-bath, under water, avoids on the one hand triangular flask to be subject to water buoyancy unstable and topple over, and causes sample to disappear to boil failure and disappear to boil liquid heavy corrosion instrument.Also can avoid on the other hand triangular flask to immerse that the water yield is how many and difference is boiled in disappearing of causing, atmospheric steam heating-up temperature is even, steam heat is high compared with boiling water, sample disappear boil more abundant, under atmospheric steam heating condition, measurement result is directly utilized the computing formula of organic carbon in GB, without other correction coefficient.
The inventive method is simple, and heating condition is easy to control, safe and efficient, and testing result accurately and reliably, is particularly useful for batch sample and detects, for the work such as nutrition diagnosis, carbon remittance research provide believable data.
Claims (10)
1. a Plants, soil organic matter detection method, the method is that plant sample or pedotheque are carried out to pre-service, by the pre-service plant sample of pre-service gained or pre-service pedotheque, potassium bichromate solution, concentrated sulfuric acid solution three is placed in triangular flask and mixes, oxidation reaction is carried out in heating, after finishing, reaction adds distilled water, cooling rear interpolation phenanthroline solution is as indicator, then use the remaining potassium dichromate of copperas solution titration oxidation reaction, calculate organic carbon content, it is characterized in that: described oxidation reaction is to react 20～60 minutes under the atmospheric steam condition producing at 90～100 ℃ of water.
2. plant according to claim 1, soil organic matter detection method, is characterized in that: described oxidation reaction is to react 30 minutes under the atmospheric steam condition producing at 96～100 ℃ of water.
3. plant according to claim 1, soil organic matter detection method, it is characterized in that: described plant sample was through 60～80 ℃ of bakings 8～48 hours, pulverized 0.25mm sieve, through 65～100 ℃, dry to constant weight and make pre-service plant sample, every 20mg～35mg pre-service plant sample need add 8ml～15mL potassium bichromate solution and 8ml～15mL concentrated sulfuric acid solution, and the potassium bichromate solution wherein adding and concentrated sulfuric acid solution volume ratio are 1:1.
4. plant according to claim 1, soil organic matter detection method, it is characterized in that: described pedotheque through air-dry removal of impurities, ground 2mm sieve, by inquartation, get 2/4 sample of crossing after 2mm sieve, grind again 0.25mm sieve series and obtained pre-service pedotheque, every 100～800mg pre-service pedotheque need add 5ml～10mL potassium bichromate solution solution and 5ml～10mL concentrated sulfuric acid solution, and the potassium bichromate solution wherein adding and concentrated sulfuric acid solution volume ratio are 1:1.
5. according to claim 1 to 4 arbitrary described plant, soil organic matter detection method, it is characterized in that: described potassium bichromate solution concentration is 0.6mol/L～1.0mol/L; Described concentrated sulfuric acid solution massfraction is 98%.
6. plant according to claim 5, soil organic matter detection method, is characterized in that: described potassium bichromate solution optimum concentration is 0.8mol/L.
7. plant according to claim 5, soil organic matter detection method, is characterized in that: described pre-service plant sample or pre-service pedotheque, concentrated sulfuric acid solution, potassium bichromate solution three remaining potassium bichromate solution after oxidation reaction is all used the titration of 0.1mol/L～0.6mol/L copperas solution.
8. plant according to claim 7, soil organic matter detection method, it is characterized in that: described pre-service plant sample, concentrated sulfuric acid solution, potassium bichromate solution three be the copperas solution titration of remaining potassium bichromate solution after oxidation reaction, described copperas solution optimum concentration is 0.4mol/L; Described pre-service pedotheque, concentrated sulfuric acid solution, potassium bichromate solution three be the copperas solution titration of remaining potassium bichromate solution after oxidation reaction, and described copperas solution optimum concentration is 0.2mol/L.
9. the heating arrangement that plant, soil organic matter detection method are used according to claim 1, described heating arrangement is comprised of thermostat water bath, spacer for hanger and capping, described thermostat water bath comprises tank, tank is provided with capping and seals, described capping top is provided with handle, it is characterized in that: on described spacer for hanger, have some eyelets, spacer for hanger is horizontally set in tank, described spacer for hanger has 1/2nd to 2/3rds tank height apart from bottom of gullet, and spacer for hanger is higher than water level in tank.
10. heating arrangement according to claim 9, is characterized in that: described capping is that the degree of depth is the iron square groove of 4～6 centimetres, and four edges of described iron square groove notch are equipped with rubber strip, and the notch edge of iron square groove presses on the notch edge of tank.
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