CN106645460B - A method of quick, Accurate Determining biogas slurry sulfite root, sulfate radical, thiosulfate anion - Google Patents
A method of quick, Accurate Determining biogas slurry sulfite root, sulfate radical, thiosulfate anion Download PDFInfo
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Abstract
The present invention relates to a kind of quick, Accurate Determining biogas slurry sulfite root, sulfate radical, thiosulfate anion methods, first prepare SO respectively3 2‑、SO4 2‑、S2O3 2‑Dan Biao, it is qualitative according to retention time, then prepare SO3 2‑、SO4 2‑、S2O3 2‑Mixed mark, obtain the linear equation of concentration and peak area, then mud sample is pre-processed to obtain biogas slurry, by treated, biogas slurry crosses 0.22 μm of polyethersulfone membranes, laggard ion chromatography is diluted with ultrapure water, column oven temperature setting is 35 DEG C, and sample volume is 20 μ l, flow velocity is 0.7ml/min, with 3.2mMNa2CO3、1.0mMNaHCO3, 20% acetone be leacheate, SO in biogas slurry is obtained according to linear equation3 2‑、SO4 2‑、S2O3 2‑Concentration.Analytic process of the present invention is completed in 30min, accuracy height, favorable reproducibility, to determine that the material stream of sulfur-containing compound provides detection means.
Description
Technical field
The present invention relates to quantitative determination sludge biogas slurry sample sulfite root, sulfate radical, thiosulfuric acid radical content method,
More particularly to a kind of quick, Accurate Determining biogas slurry sulfite root, sulfate radical, thiosulfate anion method, belong to analytical chemistry
Field.
Background technique
In recent years, malodor problem caused by sewage treatment plant has been to be concerned by more and more people.Wherein, in anaerobic digestion
The hydrogen sulfide generated in the process plays significant contribution in terms of leading to stench, and it can cause important bad shadow to human health
It rings.Studies have shown that the sulfate reduction approach in anaerobic digestion process is to generate the important channel of hydrogen sulfide.In anaerobic environment
Under, sulfate generates the weight such as sulphite, thiosulfate under the action of sulfate reducing bacteria, by a series of enzymatic reactions
Intermediate product is wanted, hydrogen sulfide is finally reduced to and discharges into atmospheric environment.Therefore, key in sulfate-reducing process is specified to contain
The variation of sulfur material, the generation for subsequent control hydrogen sulfide provide theoretical foundation, it is necessary to it is dirty to establish effective method quantitative detection
Sulfate radical, inferior sulfate radical, thiosulfate anion in mire liquid.However currently, to sulfate radical, inferior sulfate radical, sulphur in biogas slurry sample
The report of thiosulfuric acid root focuses mostly on to be measured respectively in general chemical method, and interference is big, time-consuming, poor reproducibility.Therefore, it is badly in need of building
A kind of vertical quick, sulfate radical, inferior sulfate radical, thiosulfate anion in Accurate Determining biogas slurry method.
Summary of the invention
The contents of the present invention are to solve the problems, such as the measurement of biogas slurry sample sulfite root, sulfate radical, thiosulfate anion, mention
For a kind of quick, Accurate Determining biogas slurry sulfite root, sulfate radical, thiosulfate anion method.Analysis time of the invention is short, grasps
Make easy, accuracy height, favorable reproducibility, the measurement of sulfur-bearing inorganic ions suitable for biogas slurry during anaerobic sludge digestion is full
The testing requirements of sufficient analytical chemistry.
To achieve the goals above, the present invention adopts the following technical scheme:
Quick, Accurate Determining biogas slurry sulfite root, sulfate radical, thiosulfate anion method proposed by the present invention, specifically
Steps are as follows:
(1) reagent prepares:
Leacheate: accurately weighing the carbonate reagent 16.9548g that drying to constant weight, sodium bicarbonate reagent 4.2005g, uses
Ultrapure water is settled to 500ml and leacheate stock solution is made；10ml leacheate stock solution, 200ml acetone soln are taken, is settled to
The leacheate of containing sodium carbonate 3.2mM, sodium bicarbonate 1.0mM and acetone 20% is made in 1000ml；
10MNaOH solution: accurately weighing 40gNaOH, is dissolved with ultrapure water, and in 100ml volumetric flask constant volume；
Deploy ultrapure water: prior to 2ml formalin is added in 2L volumetric flask, with ultrapure water constant volume, then with 10MNaOH solution
PH=8.0 are adjusted, obtaining pH value is 8.0, the ultrapure water containing formaldehyde 0.1%；
SO3 2-、SO4 2-、S2O3 2-Standard reserving solution: Na is accurately weighed2SO3Reagent 1.2494g adds 1ml formalin, with tune
It is settled to 1000ml with ultrapure water, the SO of 1000mg/l is made3 2-Standard reserving solution；Accurately weigh Na2SO4 2-Reagent 1.4790g,
It is settled to 1000ml after being dissolved with ultrapure water, the SO of 1000mg/l is made4 2-Standard reserving solution；Accurately weigh Na2S2O3Reagent
The S of 1000mg/l is made with 1000ml is settled to after allotment ultrapure water dissolution in 1.4107g2O3 2-Standard reserving solution；
Single mark standard solution:
Accurately pipette 1ml SO3 2-、SO4 2-、S2O3 2-Standard Stock solutions are respectively placed in 3 100ml volumetric flasks, with tune
It is settled to graduation mark with ultrapure water, obtains single mark standard solution of 10mg/l；It is dilute again
5 times are released, required SO is obtained3 2-、SO4 2-、S2O3 2-Single mark standard solution；
Mixed mark standard solution:
Accurately pipette the SO of 1ml3 2-, 2ml SO4 2-, 1ml S2O3 2-Standard reserving solution in 1 100ml volumetric flask, and
Graduation mark is settled to allotment ultrapure water；Successively accurately pipette 0.25,0.5,1,2,3,4,5ml SO3 2-、SO4 2-And S2O3 2-Group
At above-mentioned first time dilute solution be settled to graduation mark in 7 10ml volumetric flasks, and with allotment ultrapure water, obtain needed for
0.25-0.50-0.25、0.50-1.0-0.50、1.0-2.0-1.0、2.0-4.0-2.0、3.0-6.0-3.0、4.0-8.0-4.0、
The SO of 5.0-10.0-5.0mg/l3 2-、SO4 2-、S2O3 2-Mixed mark standard solution；
(2) SO3 2-、SO4 2-、S2O3 2-The analysis of mixed mark standard solution
It is qualitative: respectively by SO3 2-、SO4 2-、S2O3 2-In single mark standard solution injection ion chromatography, corresponding ion appearance is obtained
Retention time, various ions are determined according to retention time；
Repeatability: to mixed standard solution continuous sample introduction 6 times of 2.0mg/l, SO is obtained3 2-、SO4 2-、S2O3 2-Peak area
Relative standard deviation, wherein used in data processing method be calculate corrector factor method；
Linear relationship: 0.25-0.50-0.25,0.50-1.0-0.50 obtained to step (1), 1.0-2.0-1.0,
The SO of 2.0-4.0-2.0,3.0-6.0-3.0,4.0-8.0-4.0,5.0-10.0-5.0mg/l3 2-、SO4 2-、S2O3 2-Hybrid standard
Solution carries out sample introduction according to concentration from low to high, obtains the linear equation of concentration and peak area, wherein at used data
Reason method is to calculate corrector factor method；
Detection limit: it is calculated separately with 3 times of signal-to-noise ratio by SO3 2-、SO4 2-、S2O3 2-Detection limit；
Quantitative limit: SO is calculated separately with 10 times of signal-to-noise ratio3 2-、SO4 2-、S2O3 2-Quantitative limit；
(3) pretreatment of biogas slurry sample
Take mud sample 40ml in 50ml centrifuge tube, be added protective agent immediately, and with 10MNaOH tune pH=8.0(±
0.1) 5min, is shaken under 200 revs/min, then, is centrifuged 15min under the conditions of 10000r and is obtained biogas slurry, biogas slurry crosses 0.22 μm
Polyethersulfone membranes are saved in 4 DEG C of refrigerators；
(4) ion chromatography can be injected after biogas slurry sample allotment ultrapure water dilution suitable multiple after pretreatment, according to
The linear equation that step (2) obtains determines wherein SO3 2-、SO4 2-、S2O3 2-Content；
In the present invention, what ion chromatography used protect protects for 4/5 Guard/4.0 of Metrosep A SUPP, color
Spectrum column is 4/5 Guard/4.0 splitter of Metrosep A SUPP, and filler internal diameter is 5 μm, and column oven temperature setting is 35
DEG C, sample volume is 20 μ l, flow velocity 0.7ml/min, with 3.2mMNa2CO3、1.0mMNaHCO3, 20% acetone be leacheate.
In the present invention, protective agent described in step (3) is 400 μ l formaldehyde.
The beneficial effects of the present invention are:
Inferior sulfate radical, sulfate radical, thiosulfuric acid radical content in Simultaneous Determination biogas slurry of the invention, analysis
Time is short, easy to operate, accuracy is high, favorable reproducibility, the sulfur-bearing inorganic ions suitable for biogas slurry during anaerobic sludge digestion
Measurement, meet the testing requirements of analytical chemistry.
Detailed description of the invention
Fig. 1 is inferior sulfate radical, sulfate radical, thiosulfate anion standard chromatogram；Chromatographic peak (mg/l): 1. SO3 2-、
2.SO4 2-、3.S2O3 2-；
Fig. 2 is ion concentration of inferior sulfate radical and peak area linear relationship chart；
Fig. 3 is sulfate ion concentration and peak area linear relationship chart；
Fig. 4 is thiosulfate ion concentration and peak area linear relationship chart；
Fig. 5 is biogas slurry sample sulfite root, sulfate radical, thiosulfate anion concentration and peak area linear relationship chart；Chromatography
Peak (mg/l): 1. SO3 2-、2.SO4 2-、3.S2O3 2-。
Specific embodiment
It is specifically described below with reference to embodiment is bright to this law.
Instrument used in embodiment and reagent:
883 Basic ion chromatography of Metrohm；Suppressor；Electric conductivity detector；Metrosep A SUPP 4/5Guard/
4.0 guard column；4/5 Guard/4.0 splitter of Metrosep A SUPP；0.22 μm of polyether sulfone syringe filter；Moisture content
96% sludge (Quyang sewage treatment plant)；Sodium carbonate (AR grades)；Sodium bicarbonate (AR grades)；Sodium hydroxide (AR grades)；Sodium sulfite
(GR grades)；Sodium sulphate (GR grades)；Sodium thiosulfate (GR grades)；Acetonitrile (chromatographic grade)；Acetone (chromatographic grade)；Flow velocity 0.7ml/min.
Embodiment 1:
(1) reagent prepares
Leacheate: accurately weighing the carbonate reagent 16.9548g that drying to constant weight, sodium bicarbonate reagent 4.2005g, uses
Ultrapure water is settled to 500ml and leacheate stock solution is made；10ml leacheate stock solution, 200ml acetonitrile solution are taken, is settled to
The leacheate of containing sodium carbonate 3.2mM, sodium bicarbonate 1.0mM, acetonitrile 20% is made in 1000ml；Take 10ml leacheate stock solution,
200ml acetone soln, is settled to 1000ml, and the leacheate of containing sodium carbonate 3.2mM, sodium bicarbonate .0mM, acetone 20% is made；
It is selected respectively containing 20% acetonitrile, the 3.2mM sodium carbonate of 20% acetone, 1.0mM sodium bicarbonate solution as leacheate, it is right
Hybrid standard product are measured.Under the chromatographic condition of 20% acetonitrile, SO3 2-And SO4 2-Not up to baseline separation, separating degree are small
In 1.5, the accurate quantitative analysis in actual sample is influenced.Under the chromatographic condition of 20% acetone, SO3 2-、SO4 2-And S2O3 2-Realize base
Line separation, SO3 2-And SO4 2、-SO4 2-And S2O3 2-Separating degree be respectively 7.5,14.5, while SO3 2-、SO4 2-And S2O3 2-?
Appearance process is completed in 30min.Therefore the 3.2mM sodium carbonate containing 20% acetone, 1.0mM sodium bicarbonate solution is selected to be used as elution
Liquid, SO3 2-、SO4 2-And S2O3 2-Three kinds of ions do not interfere mutually, and analysis time is shorter.Under the conditions of this leacheate, to 2mg/l
SO3 2-、4mg/lSO4 2-And 2mg/lS2O3 2-Hybrid standard product are analyzed, and the chromatogram of Fig. 1 is obtained.
SO3 2-、SO4 2-、S2O3 2-Standard reserving solution: Na is accurately weighed2SO3Reagent 1.2494g adds 1ml formalin, with tune
It is settled to 1000ml with ultrapure water, the SO of 1000mg/l is made3 2-Standard reserving solution；Accurately weigh Na2SO4 2-Reagent 1.4790g,
It is settled to 1000ml after being dissolved with ultrapure water, the SO of 1000mg/l is made4 2-Standard reserving solution；Accurately weigh Na2S2O3Reagent
The S of 1000mg/l is made with 1000ml is settled to after allotment ultrapure water dissolution in 1.4107g2O3 2-Standard reserving solution；
Single mark standard solution: 1ml SO is accurately pipetted3 2-、SO4 2-、S2O3 2-Standard Stock solutions are respectively placed in 3 100ml
In volumetric flask, it is settled to graduation mark with allotment ultrapure water, obtains single mark standard solution of 10mg/l；5 times are diluted again, needed for obtaining
Single mark standard solution；
Mixed mark standard solution: the SO of 1ml is successively accurately pipetted3 2-, 2ml SO4 2-, 1ml S2O3 2-Standard reserving solution is in 1
In a 100ml volumetric flask, and graduation mark is settled to allotment ultrapure water.Successively accurately pipette 0.25,0.5,1,2,3,4,5ml
SO3 2-、SO4 2-、S2O3 2-Above-mentioned first time dilute solution is settled to scale in 7 10ml volumetric flasks, and with allotment ultrapure water
Line, obtain required 0.25-0.50-0.25,0.50-1.0-0.50,1.0-2.0-1.0,2.0-4.0-2.0,3.0-6.0-3.0,
The mixed standard solution of 4.0-8.0-4.0,5.0-10.0-5.0mg/l；
(2) SO3 2-、SO4 2-、S2O3 2-Standard solution analysis
It is qualitative: respectively by SO3 2-、SO4 2-、S2O3 2-Three kinds of single mark standard solution sample introductions, obtain ionic species and retention time
Relationship, SO3 2-、SO4 2-、S2O3 2-Retention time be respectively 12.27,15.19 and 22.65min.
Repeatability: to mixed standard solution continuous sample introduction 6 times of 2.0mg/l, SO is obtained3 2-、SO4 2-、S2O3 2-Peak area
Relative standard deviation be respectively 1.55%, 1.39% and 1.39%.
It is linear: 0.25-0.50-0.25,0.50-1.0-0.50,1.0-2.0-1.0,2.0-4.0- that step 1 is obtained
2.0, the SO of 3.0-6.0-3.0,4.0-8.0-4.0,5.0-10.0-5.0mg/l3 2-、SO4 2-、S2O3 2-Mixed standard solution is pressed
Sequence sample introduction from low to high, obtains SO under various concentration3 2-、SO4 2-、S2O3 2-Peak area, respectively with SO3 2-、SO4 2-、S2O3 2-
Concentration (mg/l) be abscissa, using its peak area be ordinate mapping, obtain SO3 2-、SO4 2-、S2O3 2-Linear equation difference
For y=0.1726x-0.0134, y=0.4075x-0.0579, y=0.3153x-0.0247, SO3 2-、SO4 2-、S2O3 2-Linear phase
Relationship number is respectively 0.9991,0.9993,0.9993.As shown in Figure 2, Figure 3, Figure 4.
Detection limit: it is calculated separately with 3 times of signal-to-noise ratio by SO3 2-、SO4 2-、S2O3 2-Detection limit, respectively 0.05,0.02,
0.04mg/l。
Quantitative limit: SO is calculated separately with 10 times of signal-to-noise ratio3 2-、SO4 2-、S2O3 2-Quantitative limit, respectively 0.17,0.08,
0.13mg/l。
(3) pretreatment of biogas slurry sample
Take mud sample 40ml in 50ml centrifuge tube, be added protective agent immediately, and with 10MNaOH tune pH=8.0(±
0.1) 5min, is shaken under 200r, then, is centrifuged 15min under the conditions of 10000r and is obtained biogas slurry, biogas slurry crosses 0.22 μm of polyether sulfone
Filter membrane is saved in 4 DEG C of refrigerators；
(4) SO in biogas slurry sample3 2-、SO4 2-、S2O3 2-The measurement of content
Chromatographic condition are as follows: what ion chromatography used protect protects for 4/5 Guard/4.0 of Metrosep A SUPP,
Chromatographic column is 4/5 Guard/4.0 splitter of Metrosep A SUPP, and filler internal diameter is 5 μm；Column oven temperature setting is
35℃；Sample volume is 20 μ l；Flow velocity is 0.7ml/min；With 3.2mMNa2CO3、1.0mMNaHCO3, 20% acetone be leacheate.
Under above-mentioned chromatographic condition, biogas slurry sample is detected, obtains SO in sludge biogas slurry3 2-、SO4 2-、S2O3 2-Ion
Detection spectrogram, see Fig. 5.According to external standard method to SO in biogas slurry3 2-、SO4 2-、S2O3 2-The concentration of ion is quantified, and biogas slurry is obtained
SO in sample3 2-、SO4 2-、S2O3 2-The content of ion, the results are shown in Table 1.It is separately added into standard solution in the sample, using mark-on
Method carries out rate of recovery experiment, and the rate of recovery the results are shown in Table 1.
Table 1
Claims (1)
1. a kind of quick, Accurate Determining biogas slurry sulfite root, sulfate radical, thiosulfate anion method, it is characterised in that specific
Steps are as follows:
(1) reagent prepares:
Leacheate: accurately weighing the carbonate reagent 16.9548g that drying to constant weight, sodium bicarbonate reagent 4.2005g, and use is ultrapure
Water is settled to 500ml and leacheate stock solution is made；10ml leacheate stock solution, 200ml acetone soln are taken, 1000ml is settled to,
The leacheate of containing sodium carbonate 3.2mM, sodium bicarbonate 1.0mM and acetone 20% is made；
10MNaOH solution: accurately weighing 40gNaOH, is dissolved with ultrapure water, and in 100ml volumetric flask constant volume；
Deploy ultrapure water: prior to 2ml formalin is added in 2L volumetric flask, with ultrapure water constant volume, then with 10MNaOH solution tune pH
=8.0, obtaining pH value is 8.0, the ultrapure water containing formaldehyde 0.1%；
SO3 2-、SO4 2-、S2O3 2-Standard solution: Na is accurately weighed2SO3Reagent 1.2494g adds 1ml formalin, ultrapure with deploying
Water is settled to 1000ml, and the SO of 1000mg/l is made3 2-Standard reserving solution；Accurately weigh Na2SO4Reagent 1.4790g, uses ultrapure water
It is settled to 1000ml after dissolution, the SO of 1000mg/l is made4 2-Standard reserving solution；Accurately weigh Na2S2O3Reagent 1.4107g is used
It is settled to 1000ml after allotment ultrapure water dissolution, the S of 1000mg/l is made2O3 2-Standard reserving solution；
Single mark standard solution:
Accurately pipette 1ml SO3 2-、SO4 2-、S2O3 2-Standard Stock solutions are respectively placed in 3 100ml volumetric flasks, super with allotment
Pure water is settled to graduation mark, obtains single mark standard solution of 10mg/l；5 times are diluted again, obtain required SO3 2-、SO4 2-、S2O3 2-It is single
Mark standard solution；
Mixed mark standard solution:
Accurately pipette the SO of 1ml3 2-, 2ml SO4 2-, 1ml S2O3 2-Standard reserving solution in 1 100ml volumetric flask, and with adjust
Graduation mark is settled to ultrapure water；Successively accurately pipette the SO of 0.25,0.5,1,2,3,4,5ml3 2-、SO4 2-And S2O3 2-Composition
First time dilute solution be settled to graduation mark in 7 10ml volumetric flasks, and with allotment ultrapure water, obtain required 0.25-
0.50-0.25、0.50-1.0-0.50、1.0-2.0-1.0、2.0-4.0-2.0、3.0-6.0-3.0、4.0-8.0-4.0、5.0-
10.0-5.0mg/l SO3 2-、SO4 2-And S2O3 2-Mixed mark standard solution；
(2) SO3 2-、SO4 2-、S2O3 2-The analysis of mixed mark standard solution
It is qualitative: respectively by SO3 2-、SO4 2-And S2O3 2-In single mark standard solution injection ion chromatography, the guarantor of corresponding ion appearance is obtained
The time is stayed, various ions are determined according to retention time；
Repeatability: to mixed mark standard solution continuous sample introduction 6 times of 2.0mg/l, SO is obtained3 2-、SO4 2-And S2O3 2-Peak area phase
To standard deviation, wherein used data processing method is to calculate corrector factor method；
Linear relationship: to step (1) obtained 0.25-0.50-0.25,0.50-1.0-0.50,1.0-2.0-1.0,2.0-
The SO of 4.0-2.0,3.0-6.0-3.0,4.0-8.0-4.0,5.0-10.0-5.0mg/l3 2-、SO4 2-、S2O3 2-Mixed mark standard is molten
Liquid carries out sample introduction according to concentration from low to high, obtains the linear equation of concentration and peak area, wherein used data processing
Method is to calculate corrector factor method；
Detection limit: SO is calculated separately with 3 times of signal-to-noise ratio3 2-、SO4 2-、S2O3 2-Detection limit；
Quantitative limit: SO is calculated separately with 10 times of signal-to-noise ratio3 2-、SO4 2-、S2O3 2-Quantitative limit；
(3) pretreatment of biogas slurry sample
Take mud sample 40ml in 50ml centrifuge tube, be added protective agent immediately, and with the pH value 8.0 of 10MNaOH tune solution ±
0.1,5min is shaken under 200 revs/min, then, is centrifuged 15min under the conditions of 10000r and is obtained biogas slurry, biogas slurry crosses 0.22 μm
Polyethersulfone membranes are saved in 4 DEG C of refrigerators；The protective agent is 400 μ l formaldehyde；
(4) ion chromatography is injected after biogas slurry sample after pretreatment allotment ultrapure water dilution suitable multiple, according to step (2)
Obtained linear equation determines wherein SO3 2-、SO4 2-、S2O3 2-Content；
Wherein: the guard column that ion chromatography uses is for 4/5 Guard/4.0 guard column of Metrosep A SUPP, chromatographic column
4/5 Guard/4.0 splitter of Metrosep A SUPP, filler internal diameter are 5 μm, and column oven temperature setting is 35 DEG C, sample introduction
Amount is 20 μ l, flow velocity 0.7ml/min, with 3.2mMNa2CO3、1.0mMNaHCO3, 20% acetone be leacheate.
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| US20220113287A1 (en) * | 2020-10-09 | 2022-04-14 | Srivatsan Mohana Rangan | Methods for simultaneous quantification of anions using ion chromatography and suppressed ion conductivity |
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| CN106645460A (en) | 2017-05-10 |
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