CN109060792B - Method for determining trace lead in water by sulfydryl paper enrichment and separation colorimetric method - Google Patents
Method for determining trace lead in water by sulfydryl paper enrichment and separation colorimetric method Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004737 colorimetric analysis Methods 0.000 title claims abstract description 14
- 238000000926 separation method Methods 0.000 title claims abstract description 12
- 125000003396 thiol group Chemical class [H]S* 0.000 claims abstract description 73
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 229960000583 acetic acid Drugs 0.000 claims abstract description 4
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 4
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000741 silica gel Substances 0.000 claims description 22
- 229910002027 silica gel Inorganic materials 0.000 claims description 22
- 239000002699 waste material Substances 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000011161 development Methods 0.000 claims description 7
- -1 hydrosulphonyl Chemical group 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000007853 buffer solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000003995 emulsifying agent Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 241000220317 Rosa Species 0.000 claims description 2
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- 230000035945 sensitivity Effects 0.000 abstract description 4
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- 239000000523 sample Substances 0.000 description 18
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 9
- 238000000502 dialysis Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 5
- 235000013361 beverage Nutrition 0.000 description 5
- 229910052793 cadmium Inorganic materials 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000000661 sodium alginate Substances 0.000 description 5
- 235000010413 sodium alginate Nutrition 0.000 description 5
- 229940005550 sodium alginate Drugs 0.000 description 5
- UOFGSWVZMUXXIY-UHFFFAOYSA-N 1,5-Diphenyl-3-thiocarbazone Chemical compound C=1C=CC=CC=1N=NC(=S)NNC1=CC=CC=C1 UOFGSWVZMUXXIY-UHFFFAOYSA-N 0.000 description 4
- 231100000331 toxic Toxicity 0.000 description 4
- 230000002588 toxic effect Effects 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000012521 purified sample Substances 0.000 description 2
- CZCBTSFUTPZVKJ-UHFFFAOYSA-N rose oxide Chemical compound CC1CCOC(C=C(C)C)C1 CZCBTSFUTPZVKJ-UHFFFAOYSA-N 0.000 description 2
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 description 1
- IICCLYANAQEHCI-UHFFFAOYSA-N 4,5,6,7-tetrachloro-3',6'-dihydroxy-2',4',5',7'-tetraiodospiro[2-benzofuran-3,9'-xanthene]-1-one Chemical compound O1C(=O)C(C(=C(Cl)C(Cl)=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 IICCLYANAQEHCI-UHFFFAOYSA-N 0.000 description 1
- 208000002109 Argyria Diseases 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 description 1
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 description 1
- 235000010703 Modiola caroliniana Nutrition 0.000 description 1
- 244000038561 Modiola caroliniana Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012470 diluted sample Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 239000003621 irrigation water Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- DNHVXYDGZKWYNU-UHFFFAOYSA-N lead;hydrate Chemical compound O.[Pb] DNHVXYDGZKWYNU-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000003969 polarography Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229930187593 rose bengal Natural products 0.000 description 1
- 229940081623 rose bengal Drugs 0.000 description 1
- STRXNPAVPKGJQR-UHFFFAOYSA-N rose bengal A Natural products O1C(=O)C(C(=CC=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 STRXNPAVPKGJQR-UHFFFAOYSA-N 0.000 description 1
- 229930007790 rose oxide Natural products 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1813—Specific cations in water, e.g. heavy metals
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for determining trace lead in water by a mercapto paper enrichment and separation colorimetric method, which comprises the following steps: the method comprises the steps of (1) preparing mercapto grafting solution, adding 60.0ml of thioglycollic acid, 36.0ml of acetic anhydride, 24.0ml of glacial acetic acid and 10 drops of concentrated sulfuric acid, shaking up, sealing and storing in a dark place; and (4) developing the sulfydryl paper analytic solution enriched with the lead in the water, and detecting. The method provided by the invention has high enrichment ratio, does not need washing operation in determination, overcomes the problem that the washing operation in the hydrosulfuryl cotton enrichment method causes dilution of a sample, and improves the sensitivity of the test.
Description
Technical Field
The invention belongs to the field of environmental detection, and particularly relates to a method for determining trace lead in water by a mercapto paper enrichment and separation colorimetric method.
Background
The existing method for measuring trace lead in environmental water comprises a dithizone colorimetric method, an atomic absorption photometry, a polarography method, an atomic fluorescence method and the like, wherein some methods need expensive instruments, some analysis steps are complex, and more importantly, some methods need toxic solvent extraction and highly toxic potassium cyanide is used as a masking agent. Recently, the method for measuring lead by using sodium rosette instead of dithizone is reported, the lead and the sodium rosette react to generate a stable mauve complex, the mass concentration of the lead is in the range of 8mg/L-20mg/L and accords with the beer law, the maximum absorption wavelength is 546nm, and the expression molar coefficient is 1.50x104And the determination result of the sample with the recovery rate of 96.8-104 percent has no obvious difference from the national standard dithizone method. However, the lead concentration in the water is 8mg/L at the most limit, the heavy metal lead in the water is limited, the domestic water is limited to 0.2mg/L, and the agricultural water is 0.3mg/L, so that the direct determination of the lead in the water by the sodium rose oxide is impossible, and the lead must be enriched and separated.
The enrichment technology adopted at present is a ring furnace technology and a sulfhydryl carrier technology, wherein the ring furnace technology is complex and time-consuming to operate, the sulfhydryl carrier technology comprises sulfhydryl cotton, sulfhydryl resin, sulfhydryl carbon and the like, and the technologies need grafting, equipment preparation and rinsing, so that the determination sensitivity is reduced.
Through search, the patent literature relevant to the present application discloses the following:
CN104048959B discloses an ultra-trace lead and cadmium ion detection method, which comprises the following steps: (1) carrying out acidification treatment on a sample to be detected: adding hydrochloric acid or nitric acid into a sample to be detected, and adjusting the pH value of the sample to be detected to be between 1 and 4 to obtain an acidified sample; (2) removing Hg from the acidified sample obtained in step (1)2+And Zn2+Obtaining a purified sample; (3) diluting the purified sample obtained in the step (2) with a buffer solution, and adjusting the pH value of the diluted sample to be between 6 and 9 to obtain a neutral sample; (4) contacting the neutral sample obtained in the step (3) with dithizone to react to generate a lead-cadmium ion-dithizone complex; (5) adding a sulfide solution into the lead-cadmium ion-dithizone complex generated in the step (4) to enable the lead-cadmium ion-dithizone complex to completely react to generate PbS and/or CdS, and obtaining a mixture containing PbS and/or CdS; (6) and (3) carrying out silver staining reaction on the mixture containing PbS and/or CdS obtained in the step (5) for 5-30 minutes to obtain a reaction product, and determining the concentration of lead and cadmium ions in the sample to be detected according to the gray level of the reaction product and the principle that the concentration of lead and cadmium ions in the sample to be detected is higher when the gray level value is larger.
CN105823668A discloses a method for nonequilibrium enrichment and measurement of ultra-trace lead and cadmium ions in a beverage, which comprises the following steps: 1) pretreating the binding agent, preparing a dialysis bag by using a cellulose acetate dialysis membrane, filling the binding agent sodium alginate into the dialysis bag, and soaking in deionized water for 12-72 h for purification; 2) the collection device is installed to prepare purified sodium alginate into 0.001-0.005 mol/L sodium alginate aqueous solution, the sodium alginate solution is measured according to the volume of the collection device and is loaded into the collection device, and the collection device is sealed by a cellulose acetate dialysis membrane; 3) placing the acquisition device filled with the sodium alginate binding agent in the liquid beverage for 24-240 h, wherein the dialysis membrane of the acquisition device is downward during placement, and then fixing the acquisition device; 4) taking out the collecting devices, detecting and taking out the collecting devices, taking out the binding agent enriched with lead ions and cadmium ions in each collecting device according to 50-80% of the total volume, fixing the volume with 1-2% of nitric acid, and measuring the accumulation amount of the lead ions and the cadmium ions in the binding agent; 5) calculating the concentration of lead and cadmium ions in the beverage according to a formula CM (M · Δ g/D · t · A), and calculating the concentration of heavy metal cations in the beverage; in the formula, CM is the concentration of lead ions or cadmium ions in the beverage, M is the accumulation amount of lead or cadmium in the binding agent, Δ g is the thickness of the dialysis membrane, D is the diffusion coefficient of the lead ions or cadmium ions through the dialysis membrane, t is the diffusion time, and A is the working area of the dialysis membrane.
The patent does not disclose a detailed description of related materials for measuring trace lead in water, and the patent develops a sulfydryl paper enrichment device, so that the device can be used for carrying out high-rate enrichment on water, can directly measure the trace lead without rinsing, has high sensitivity and simple method, and completely meets the requirements of measuring the trace lead in domestic water and irrigation water.
Disclosure of Invention
Aiming at the technical requirements and the current situation of the current environment-friendly method for enriching, separating and measuring heavy metal lead in water, the invention provides the method for measuring trace lead in water by the sulfydryl paper enrichment and separation colorimetric method, which has the advantages of simplicity, high enrichment ratio, no need of leaching and environment-friendly discharge of detection residual liquid.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for determining trace lead in water by a mercapto paper enrichment and separation colorimetric method comprises the following steps:
preparation of mercapto paper
(1) Sulfydryl grafting liquid
Adding 60.0ml thioglycollic acid, 36.0ml acetic anhydride, 24.0ml glacial acetic acid and 10 drops of concentrated sulfuric acid, shaking up, sealing and storing in dark place;
(2) mercapto grafting
Immersing medium-speed qualitative filter paper strips into the sulfydryl grafting solution for 24 hours;
secondly, taking out the filter paper strips, shaking and cleaning the filter paper strips in distilled water for 10min, then shaking and cleaning the filter paper strips in clean distilled water for 10min, and taking out the filter paper strips to be protected from light and dried;
flattening the dried mercapto-group paper strips, and cutting the mercapto-group paper strips into round pieces by using a shaper for later use;
secondly, the prepared sulfhydryl paper is put into a sulfhydryl paper fixer in a simple device for enriching lead in water by the sulfhydryl paper for testing, and the testing method is as follows:
enriching
Placing a funnel with a mercapto-based paper fixer at the bottom on a waste liquid collector;
injecting 200ml of the predicted water sample into a funnel, controlling the flow rate within 30ml/min, and standing for 5min after the water sample completely flows out;
analysis of
Taking out the hydrosulphonyl paper disk enriched with lead in water, putting the disk into a colorimetric tube, adding 1ml of HCL with PH 2, soaking for 2min, and shaking continuously;
③ color development
Adding 2ml buffer solution, 1ml solubilizer, developer rose sodium solution (0.5%), 4 drops, shaking for reaction for 10 min;
colour comparison
And (3) taking the upper edge of the mercapto paper wafer out of the liquid level, attaching the wafer to the inner wall of the colorimetric tube, and comparing with a standard colorimetric plate by taking the wafer as a background to determine the content of lead in the measured water sample.
Moreover, the preparation method of the standard colorimetric plate comprises the following steps:
preparing 0,0.1, 0.2 and 0.3mg/L lead standard solution;
secondly, respectively taking 200ml of the standard solution, and respectively processing according to the first enrichment, the second analysis and the third color development in the second test step;
thirdly, the upper edge of the mercapto paper wafer is lifted out of the liquid level, the wafer is attached to the inner wall of the colorimetric tube, and the wafer is taken as the background and is respectively photographed to prepare the standard color plate.
Furthermore, the solubilizer was a 14wt% aqueous solution of emulsifier OP.
Further, the pH of the buffer solution was 7.37.
Moreover, the structure of the simple device for enriching lead in water by using the mercapto-paper is as follows: the device comprises a funnel, a mercapto paper fixer and a waste liquid collector, wherein the funnel is coaxially arranged at the upper part of the waste liquid collector, the outer edge of a lower tube of the funnel is coaxially and fixedly provided with the mercapto paper fixer, mercapto paper is embedded in the mercapto paper fixer, and the mercapto paper fixer is connected and locked with a funnel branch tube with a silica gel sleeve through threads;
the funnel is a conical glass funnel, a branch pipe is integrally formed at the lower part of the funnel, the pipe orifice of the branch pipe is a flat opening, a silica gel sleeve is coaxially sleeved outside the lower part of the branch pipe, and an external thread is formed on the outer wall of the silica gel sleeve;
the mercapto paper fixer comprises a limiting jacket, a silica gel eye ring and a tail pipe, wherein the limiting jacket is a hollow cylindrical pipe, the upper part of the inner wall of the limiting jacket is provided with an internal thread matched with the external thread of the silica gel sleeve, the lower end part of the limiting jacket is radially and inwardly integrally provided with a limiting ring, the inner diameter and the outer diameter of the tail pipe are the same as those of the branch pipe, the upper end of the tail pipe is radially and outwardly integrally provided with a positioning ring, the positioning ring is coaxially embedded on the limiting ring, the tail pipe is connected to the lower end part of the funnel branch pipe by the limiting jacket, and mercapto paper is coaxially embedded between the; a silica gel eye is coaxially arranged between the mercapto paper and the positioning ring.
Moreover, the waste liquid collecting bottle is a wide-mouth conical bottle with scales, and a protruding nozzle is arranged on one side of the bottle mouth.
And the water outlet at the lower end of the tail pipe is an inclined opening.
And the material of the limiting jacket is polyethylene.
The invention has the advantages and positive effects that:
1. the method provided by the invention is simple to operate, does not use expensive instruments, can be operated by common laboratories and individuals, and provides data for the early warning of the excessive water lead in the environment.
2. The method provided by the invention has high enrichment ratio, does not need washing operation in determination, overcomes the problem that the washing operation in the hydrosulfuryl cotton enrichment method causes dilution of a sample, and improves the sensitivity of the test.
3. The mercapto paper in the method provided by the invention can be used as a background of color comparison after enrichment, analysis and color development, so that the color comparison is easier to observe.
4. The method provided by the invention does not use toxic extractant and highly toxic cyanide masking agent in the national standard colorimetric method in the operation process, so the test solution is nontoxic and safe to operate, and the detection residual liquid can be discharged in an environment-friendly manner.
5. The method provided by the invention has good selectivity, can effectively eliminate the interference of various ions of Zn, Cd, Hg, Cr, Cu, As, Ca, Mg and the like, and has high detection accuracy and high detection precision.
Drawings
FIG. 1 is a schematic structural diagram of a simple device for enriching lead in water by using mercapto paper;
fig. 2 is a partial sectional view of a simple device for enriching lead in water by using mercapto paper.
Detailed Description
The present disclosure will be described in further detail with reference to specific examples, which are provided for illustrative purposes only and are not intended to limit the scope of the present disclosure.
A method for determining trace lead in water by a mercapto paper enrichment and separation colorimetric method comprises the following steps:
1. preparation of mercapto paper
(1) Sulfydryl grafting liquid
Adding 60.0ml thioglycollic acid, 36.0ml acetic anhydride, 24.0ml glacial acetic acid and 10 drops of concentrated sulfuric acid, shaking up, sealing and storing in dark place;
(2) mercapto grafting
Immersing the medium-speed qualitative filter paper strips into the sulfydryl grafting solution for 24 hours.
And secondly, taking out the filter paper strip, shaking and cleaning the filter paper strip in distilled water for 10min, then shaking and cleaning the filter paper strip in clean distilled water for 10min, and taking out the filter paper strip to be dried in the dark.
And thirdly, flattening the dried sulfhydryl paper strips, and cutting the strips into round pieces by using a shaper for later use.
2. The prepared sulfhydryl paper is put into a sulfhydryl paper fixer in a simple device for enriching lead in water by the sulfhydryl paper, and the test method is as follows:
enriching
A funnel with a mercapto-based paper holder at the bottom was placed on a waste liquid collector.
And (3) injecting 200ml of the predicted water sample into a funnel, controlling the flow rate within 30ml/min, and standing for 5min after the water sample completely flows out.
Analysis of
Taking out the hydrosulphonyl paper disk enriched with lead in water, putting the disk into a colorimetric tube, adding 1ml of HCL with PH 2, soaking for 2min, and shaking continuously.
③ color development
2ml of buffer solution (pH 7.37), 1ml of solubilizer, developer sodium rose bengal solution (0.5%), 4 drops and shaking were added and reacted for 10 min. The solubilizer was a 14wt% aqueous solution of emulsifier OP.
Colour comparison
The upper edge of the mercapto-paper wafer is lifted out of the liquid level, the wafer is attached to the inner wall of the colorimetric tube, and is used as a background to be compared with a standard colorimetric plate, so that the content of lead in the measured water sample is determined;
3. the preparation method of the standard colorimetric plate comprises the following steps:
preparing 0,0.1, 0.2 and 0.3mg/L lead standard solution;
collecting 200ml of the standard solution, and processing according to the steps of enrichment, analysis and color development in the test 2.
Thirdly, the upper edge of the mercapto paper wafer is lifted out of the liquid level, the wafer is attached to the inner wall of the colorimetric tube, and the wafer is taken as the background and is respectively photographed to prepare the standard color plate.
The simple device for enriching the lead in the water by the mercapto paper has the structure that the simple device comprises a funnel 1, a mercapto paper fixer 2 and a waste liquid collector 3, the funnel is coaxially arranged at the upper part of the waste liquid collector, the mercapto paper fixer is coaxially and fixedly arranged at the outer edge of the lower tube of the funnel, high-load mercapto paper 6 is embedded in the mercapto paper fixer, and the mercapto paper fixer is connected and locked with a funnel branch tube with a silica gel sleeve 5 through threads, so that the high-load mercapto paper is tightly clamped.
The funnel is toper glass funnel, and its lower part integrated system has branch pipe 4, and the branch pipe mouth of pipe is the flat mouth, and the coaxial overcoat in branch pipe lower part has the silica gel cover, and the port flushes under the lower port of silica gel cover and the branch pipe, and the outer wall system of this silica gel cover has the external screw thread.
The mercapto paper fixer comprises a limiting jacket 9, a silica gel eye ring 7 and a tail pipe 10, wherein the limiting jacket is a hollow cylindrical pipe, the upper part of the inner wall of the limiting jacket is provided with an internal thread matched with the external thread of the silica gel sleeve, the lower end part of the limiting jacket is provided with a limiting ring in a radial inward integrated mode, the inner diameter and the outer diameter of the tail pipe are the same as those of the branch pipe, the upper end of the tail pipe is provided with a positioning ring 8 in a radial outward integrated mode, the positioning ring is coaxially embedded on the limiting ring, the tail pipe is connected to the lower end part of the funnel branch pipe by the limiting jacket, mercapto paper is coaxially embedded between the lower end part of the funnel branch pipe and the positioning ring, and the silica gel sleeve is.
In order to improve the sealing performance between a tail pipe in the mercapto paper fixer and a funnel branch pipe with a silica gel sleeve, a silica gel eye is coaxially installed between the mercapto paper and a positioning ring, the inner diameter and the outer diameter of the silica gel eye are the same as those of the positioning ring, the stability of clamping the high-load mercapto paper is improved, the connection sealing performance between the branch pipe and the tail pipe is ensured, and a water sample to be tested is prevented from permeating to a connection gap when passing through the high-load mercapto paper, so that the detection result is influenced.
The waste liquid collecting bottle is a wide-mouth conical bottle with scales, and a protruding nozzle is manufactured on one side of the bottle mouth of the waste liquid collecting bottle, so that liquid filtered in the bottle can be poured conveniently, and meanwhile, when the liquid is filtered, the waste liquid collecting bottle is used as a vent, the air pressure is kept unchanged, and the normal filtering speed is maintained.
Claims (5)
1. A method for determining trace lead in water by a mercapto paper enrichment and separation colorimetric method is characterized by comprising the following steps: the method comprises the following steps:
preparation of mercapto paper
(1) Sulfydryl grafting liquid
Adding 60.0ml thioglycollic acid, 36.0ml acetic anhydride, 24.0ml glacial acetic acid and 10 drops of concentrated sulfuric acid, shaking up, sealing and storing in dark place;
(2) mercapto grafting
Immersing medium-speed qualitative filter paper strips into the sulfydryl grafting solution for 24 hours;
secondly, taking out the filter paper strips, shaking and cleaning the filter paper strips in distilled water for 10min, then shaking and cleaning the filter paper strips in clean distilled water for 10min, and taking out the filter paper strips to be protected from light and dried;
flattening the dried mercapto-group paper strips, and cutting the mercapto-group paper strips into round pieces by using a shaper for later use;
secondly, the prepared sulfhydryl paper is put into a sulfhydryl paper fixer in a simple device for enriching lead in water by the sulfhydryl paper for testing, and the testing method is as follows:
enriching
Placing a funnel with a mercapto-based paper fixer at the bottom on a waste liquid collector;
injecting 200ml of the predicted water sample into a funnel, controlling the flow rate within 30ml/min, and standing for 5min after the water sample completely flows out;
analysis of
Taking out the hydrosulphonyl paper wafer enriched with lead in water, putting the hydrosulphonyl paper wafer into a colorimetric tube, adding 1ml of HCL with PH =2, soaking for 2min, and shaking continuously;
③ color development
Adding 2ml buffer solution, 1ml solubilizer, 0.5% color reagent rose sodium solution 4 drops, shaking to react for 10 min;
colour comparison
The upper edge of the mercapto-paper wafer is lifted out of the liquid level, the wafer is attached to the inner wall of the colorimetric tube, and is used as a background to be compared with a standard colorimetric plate, so that the content of lead in the measured water sample is determined;
the solubilizer is a 14wt% aqueous solution of emulsifier OP,
pH =7.37 of the buffer solution;
the structure of the simple device for enriching lead in water by using the mercapto paper is as follows: the device comprises a funnel, a mercapto paper fixer and a waste liquid collector, wherein the funnel is coaxially arranged at the upper part of the waste liquid collector, the outer edge of a lower tube of the funnel is coaxially and fixedly provided with the mercapto paper fixer, mercapto paper is embedded in the mercapto paper fixer, and the mercapto paper fixer is connected and locked with a funnel branch tube with a silica gel sleeve through threads;
the funnel is a conical glass funnel, a branch pipe is integrally formed at the lower part of the funnel, the pipe orifice of the branch pipe is a flat opening, a silica gel sleeve is coaxially sleeved outside the lower part of the branch pipe, and an external thread is formed on the outer wall of the silica gel sleeve;
the mercapto paper fixer comprises a limiting jacket, a silica gel eye ring and a tail pipe, wherein the limiting jacket is a hollow cylindrical pipe, the upper part of the inner wall of the limiting jacket is provided with an internal thread matched with the external thread of the silica gel sleeve, the lower end part of the limiting jacket is radially and inwardly integrally provided with a limiting ring, the inner diameter and the outer diameter of the tail pipe are the same as those of the branch pipe, the upper end of the tail pipe is radially and outwardly integrally provided with a positioning ring, the positioning ring is coaxially embedded on the limiting ring, the tail pipe is connected to the lower end part of the funnel branch pipe by the limiting jacket, and mercapto paper is coaxially embedded between the; a silica gel eye is coaxially arranged between the mercapto paper and the positioning ring.
2. The method for determining trace lead in water by the thiol paper enrichment and separation colorimetry according to claim 1, wherein: the preparation method of the standard colorimetric plate comprises the following steps:
preparing 0,0.1, 0.2 and 0.3mg/L lead standard solution;
secondly, respectively taking 200ml of the standard solution, and respectively processing according to the first enrichment, the second analysis and the third color development in the second test step;
taking the upper edge of the hydrosulfuryl paper wafer out of the liquid level to make the wafer attached to the inner wall of the colorimetric tube, and taking the wafer as a background to take pictures respectively to prepare a standard colorimetric plate.
3. The method for determining trace lead in water by the thiol paper enrichment and separation colorimetry according to claim 1, wherein: the waste liquid collector is a wide-mouth conical bottle with scales, and a protruding nozzle is arranged on one side of the bottle mouth.
4. The method for determining trace lead in water by the thiol paper enrichment and separation colorimetry according to claim 1, wherein: the water outlet at the lower end of the tail pipe is an inclined opening.
5. The method for determining trace lead in water by the thiol paper enrichment and separation colorimetry according to claim 1, wherein: the limiting jacket is made of polyethylene.
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