CN112858262A - Method for rapidly detecting 19 elements in surfactant and oil chemicals - Google Patents
Method for rapidly detecting 19 elements in surfactant and oil chemicals Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 32
- 239000000126 substance Substances 0.000 title claims abstract description 19
- 230000029087 digestion Effects 0.000 claims abstract description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 13
- 239000012085 test solution Substances 0.000 claims abstract description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 230000010355 oscillation Effects 0.000 claims abstract description 6
- 230000003595 spectral effect Effects 0.000 claims abstract description 6
- 239000012224 working solution Substances 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000005259 measurement Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 40
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 34
- 239000010949 copper Substances 0.000 claims description 23
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 20
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 20
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 20
- 229910052782 aluminium Inorganic materials 0.000 claims description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 20
- 229910052796 boron Inorganic materials 0.000 claims description 20
- 229910052793 cadmium Inorganic materials 0.000 claims description 20
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 20
- 229910052742 iron Inorganic materials 0.000 claims description 20
- 229910052698 phosphorus Inorganic materials 0.000 claims description 20
- 239000011574 phosphorus Substances 0.000 claims description 20
- 229910052725 zinc Inorganic materials 0.000 claims description 20
- 239000011701 zinc Substances 0.000 claims description 20
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 19
- 239000011575 calcium Substances 0.000 claims description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 18
- 229910052791 calcium Inorganic materials 0.000 claims description 18
- 229910052749 magnesium Inorganic materials 0.000 claims description 18
- 239000011777 magnesium Substances 0.000 claims description 18
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 17
- 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 17
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 17
- 229910052788 barium Inorganic materials 0.000 claims description 17
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052804 chromium Inorganic materials 0.000 claims description 17
- 239000011651 chromium Substances 0.000 claims description 17
- 229910052759 nickel Inorganic materials 0.000 claims description 17
- 229910052700 potassium Inorganic materials 0.000 claims description 17
- 239000011591 potassium Substances 0.000 claims description 17
- 239000011734 sodium Substances 0.000 claims description 17
- 229910052708 sodium Inorganic materials 0.000 claims description 17
- 229910052712 strontium Inorganic materials 0.000 claims description 17
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 17
- 239000010936 titanium Substances 0.000 claims description 17
- 229910052719 titanium Inorganic materials 0.000 claims description 17
- 229910052720 vanadium Inorganic materials 0.000 claims description 17
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 17
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 16
- -1 polypropylene Polymers 0.000 claims description 10
- 239000004743 Polypropylene Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000000691 measurement method Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 27
- 238000011084 recovery Methods 0.000 abstract description 11
- 239000004519 grease Substances 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 6
- 239000012086 standard solution Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 235000014113 dietary fatty acids Nutrition 0.000 description 5
- 229930195729 fatty acid Natural products 0.000 description 5
- 239000000194 fatty acid Substances 0.000 description 5
- 150000004665 fatty acids Chemical class 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000000120 microwave digestion Methods 0.000 description 4
- 238000002203 pretreatment Methods 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 3
- 229910000861 Mg alloy Inorganic materials 0.000 description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 3
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 3
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 159000000009 barium salts Chemical class 0.000 description 3
- 229960003237 betaine Drugs 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000003093 cationic surfactant Substances 0.000 description 3
- BFGKITSFLPAWGI-UHFFFAOYSA-N chromium(3+) Chemical compound [Cr+3] BFGKITSFLPAWGI-UHFFFAOYSA-N 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 150000002191 fatty alcohols Chemical class 0.000 description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 159000000008 strontium salts Chemical class 0.000 description 3
- 229910001935 vanadium oxide Inorganic materials 0.000 description 3
- 238000000209 wet digestion Methods 0.000 description 3
- 239000002888 zwitterionic surfactant Substances 0.000 description 3
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 2
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 235000021360 Myristic acid Nutrition 0.000 description 2
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the field of element analysis and detection of surfactants and grease chemicals. The technical scheme is as follows: a method for rapidly detecting 19 elements in a surfactant and an oil chemical comprises the following steps: 1) accurately weighing 0.3-1.0g of uniform sample in a centrifuge tube; 2) adding 3-7mL of nitric acid into the centrifuge tube, covering the centrifuge tube, performing ultrasonic oscillation, then adding 0.2-0.6mL of hydrogen peroxide, covering the centrifuge tube, and screwing tightly; 3) digesting at the temperature of 115 ℃ and 120 ℃ in a digestion instrument; 4) taking down, cooling to room temperature, and directly fixing the volume; 5) preparing standard working solution, setting working conditions of a spectrometer instrument, selecting spectral line wavelengths of all elements, and drawing a standard curve by using an inductively coupled plasma emission spectrometer; 6) and (4) introducing the test solution obtained in the step (4) into an inductively coupled plasma emission spectrometer, and performing on a computer for measurement. The method can perform multi-element simultaneous detection, and has the advantages of high precision, high recovery rate, high detection limit, and simple operation.
Description
Technical Field
The invention belongs to the field of element analysis and detection of surfactants and grease chemicals, and particularly relates to a method for rapidly detecting 19 elements such as lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium, zinc and the like in the surfactants and the grease chemicals.
Background
China is a big country for producing and selling surfactants and grease chemicals. From 2009 to 2014, the market size of chinese surfactants has increased at a rate of 5.2% per year ("yearbook for chinese surfactant industry"). According to the statistics of the raw material and product production enterprises in 2019 by the surfactant professional committee of the national association of detergent industries, the surfactant products yield 340.77 ten thousand tons in total in 2019. The grease chemicals are mainly divided into three major categories of fatty acid, fatty alcohol and glycerin, taking the fatty acid and the fatty alcohol as examples, the total fatty acid yield in China in 2010 is 130 million tons, and the total fatty acid yield accounts for 16% of the total global yield; the total yield of fatty alcohol is 5O ten thousand tons, which accounts for 15 percent of the global yield.
The surfactant is mainly applied to daily washing and protecting products and industrial products, wherein the daily washing and protecting products account for 52 percent of the total amount, and the rest of the surfactant is mainly applied to the industrial fields of textiles, coatings, agricultural chemicals, leather papermaking, industrial cleaning, oil extraction industry and the like. The application of the oil chemicals mainly focuses on the fields of surfactants, soaps, detergents, cosmetics, emulsifiers and the like. The surfactant accounts for a high proportion of the daily care detergent ingredients. For example, in the dosage of face washes, shampoos and body washes, the surfactant comprises about 20-30%, and in creams and lotions also up to 20%. Along with the advocation of people to concepts of environmental protection, green, nature and the like, the grease-based surfactant and the grease product thereof are more and more widely applied to high-grade cosmetics. Therefore, the quality of these raw materials has a relatively large influence on the final product. In addition, ionic solutions of some elements have colors, e.g., blue for copper ions, light green for ferrous ions, light pink for manganese ions, and pink and blue-green for divalent cobalt and trivalent chromium ions, respectively, which can affect the appearance of the cosmetic product and even the final product.
The element detection mainly comprises two parts of digestion pretreatment and computer test. At present, the main digestion pretreatment methods comprise microwave digestion, wet digestion, high-pressure digestion, dry digestion and the like. Microwave digestion equipment is expensive, the requirement on cleaning a digestion container and a constant volume container is high, and the digestion container and the constant volume container are generally soaked in a nitric acid solution with the concentration of more than 5 percent for more than 24 hours; the consumption of wet digestion acid is high, ashing is easily caused in digestion and acid dispelling stages, elements are lost, and the requirement on experimental operation proficiency of experimenters is high; the high-pressure digestion has high requirements on cleaning the digestion container and the constant-volume container, and is matched with a stainless steel outer tank for use, so that time and labor are wasted; the dry digestion has high requirements on cleaning of a digestion container and a constant volume container, is suitable for only partial elements by burning a sample at high temperature, is easy to introduce external pollution and has poor detection limit. The four methods are not widely applied to the field of detection of surfactant and oil chemical elements at present. Meanwhile, for the part on the machine for measuring the metal elements in the chemical products, visual colorimetry (GB/T7532-2008 visual colorimetry for measuring heavy metals in organic chemical products), titration method (GB/T5551-2010 method for measuring the total content of calcium and magnesium ions in the surfactant dispersant) and the like are mainly adopted, and the methods are poor in reference range, detection capability and the like. In conclusion, a reliable and applicable system method is lacked in the detection method of the surfactant and the oleochemical elements.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provide a method for reliably and rapidly detecting 19 elements in a surfactant and an oil chemical, the method can carry out multi-element simultaneous detection, the precision, the recovery rate and the detection limit can meet the requirements, and the operation is simple.
The purpose of the invention is realized by the following technical scheme:
a method for rapidly detecting 19 elements in a surfactant and an oil chemical comprises the following steps:
1) accurately weighing 0.3-1.0g of uniform sample in a centrifuge tube;
2) adding 3-7mL of nitric acid into the centrifuge tube, covering the centrifuge tube, performing ultrasonic oscillation, then adding 0.2-0.6mL of hydrogen peroxide, covering the centrifuge tube, and screwing tightly;
3) digesting at the temperature of 115 ℃ and 120 ℃ in a digestion instrument;
4) taking down, cooling to room temperature, and directly fixing the volume;
5) preparing a standard working solution containing 19 elements of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc, setting the working conditions of a spectrometer instrument, selecting spectral line wavelengths of the elements, and drawing a standard curve by using an inductively coupled plasma emission spectrometer;
6) and (4) introducing the test solution obtained in the step (4) into an inductively coupled plasma emission spectrometer, and performing on-machine determination on the contents of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc in the test solution by using a peak area determination method.
A method for rapidly detecting 19 elements in a surfactant and an oil chemical comprises the following steps:
1) accurately weighing 0.3-1.0g of uniform sample in a centrifuge tube with a screw cap;
2) adding 5mL of nitric acid into the centrifuge tube, covering the centrifuge tube, performing ultrasonic oscillation for 10 minutes, adding 0.4mL of hydrogen peroxide, covering the centrifuge tube, and screwing tightly;
3) digesting for 1.5-2 hours at the temperature of 115 ℃ and 120 ℃ in a graphite digestion instrument;
4) taking down, cooling to room temperature, and directly metering to 50 mL;
5) preparing a standard working solution containing 19 elements of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc, setting the working conditions of a spectrometer instrument, selecting spectral line wavelengths of the elements, and drawing a standard curve by using an inductively coupled plasma emission spectrometer;
6) and (4) introducing the test solution obtained in the step (4) into an inductively coupled plasma emission spectrometer, and performing computer measurement on the contents of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc in the test solution by using a peak area measurement method.
The uniform sample in the step 1) comprises 0.3-0.5g of solid sample or 0.5-1.0g of liquid sample.
The centrifuge tube in the step 1) is a flat-bottom or conical-bottom 50mL polypropylene centrifuge tube.
And 6) filtering the test solution in the step 6) by using quick filter paper.
The 19 elements are lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc.
The invention has the beneficial effects that:
1. in the invention, the digestion pretreatment operation is simple, time and labor are saved, and the comprehensive cost is low.
2. The element determination method has the advantages of good repeatability, low detection limit and reliable detection data.
3. The invention has wide element detection range and can simultaneously detect 19 elements of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc. Meanwhile, the pretreatment method can also be adopted for detecting elements except 19 elements in the invention. The method can also be used for detecting related elements in food.
Detailed Description
The present invention is compared with several current main pretreatment methods as follows:
in the above table, economics are evaluated in terms of equipment, acid usage and time cost. The microwave digestion instrument and the polytetrafluoroethylene digestion tank are expensive, and the acid consumption is large; the usage amount of wet digestion acid is large, and the consumed time is long; dry digestion and high pressure digestion take a long time. The above four methods all require a lot of time for immersion cleaning of the relevant container. The pretreatment method has economical efficiency in equipment, acid use amount and time cost.
Compared with the existing main chemical product element detection method, the method disclosed by the invention has the following table:
in the table, GB/T7532-; the detection range is limited to heavy metals (lead meters). GB/T5551-2010 titration detection is only suitable for calcium and magnesium detection in water-soluble products. The ICP-OES can be used for simultaneously detecting the contents of 19 elements such as lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium, zinc and the like.
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
1. Materials and reagents
The water is first-grade water meeting the regulation in GB/T6682.
Nitric acid super grade pure
Pure hydrogen peroxide analysis
Argon (not less than 99.999 percent) or liquid argon
PP Centrifuge Tube KIRGEN 50mL Polypropylene conventional centrifugal Tube KG2811
2. Elemental standard solution: lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium, zinc (1000mg/L), using single element or multi-element standard solutions that are certified by the state and that grant a certificate of standard substance.
Preparing a standard solution: accurately absorbing a proper amount of unit element standard solution, diluting the unit element standard solution step by using a nitric acid solution (5+95) to prepare a mixed standard solution series, wherein the mass concentration of each element is as follows:
3. apparatus and device
The microwave digestion instrument, the American CEM MARSXPress, is provided with a polytetrafluoroethylene digestion inner tank.
The graphite digestion instrument of Leibetake DigiBlock ED54 is provided with a temperature programming system
PerkinElmer Optima8000 of inductive coupling plasma emission spectrometer is provided with hydrofluoric acid resistant sampling system
Ultrasonic cleaner Kunshan adhesive tape KH7200B
The electronic balance has a sensitive quantity of 0.1 mg.
4. The working conditions of the inductively coupled plasma emission spectrometer are as follows:
power: 1.20kW, plasma gas flow: 15L/min, atomizer pressure: 200kPa, auxiliary air flow rate: 1.50L/min, instrument stability delay: 15s, sample introduction time delay: 20s, number of readings: 3 times. The recommended analytical lines for each element are shown in the following table:
| element(s) | Analysis line wavelength (nm) |
| Lead (II) | 220.353 |
| Cadmium (Cd) | 228.802 |
| Chromium (III) | 267.716 |
| Aluminium | 396.153 |
| Boron | 249.677 |
| Barium salt | 233.527 |
| Calcium carbonate | 317.933 |
| Copper (Cu) | 327.393 |
| Iron | 238.204 |
| Potassium salt | 766.490 |
| Magnesium alloy | 285.213 |
| Manganese oxide | 257.610 |
| Sodium salt | 589.592 |
| Nickel (II) | 231.604 |
| Phosphorus (P) | 213.617 |
| Strontium salt | 407.771 |
| Titanium (IV) | 334.940 |
| Vanadium oxide | 292.464 |
| Zinc | 206.200 |
5. Example 1
(1) A uniform sample of 0.35g monoglyceride was accurately weighed into a 50mL polypropylene centrifuge tube (flat bottom or conical bottom) with a screw cap and graduations.
(2) Adding 5mL of nitric acid into the centrifuge tube, covering the centrifuge tube, performing ultrasonic oscillation for 10 minutes, adding 0.4mL of hydrogen peroxide, covering the centrifuge tube, and screwing.
(3) Digesting at 118 ℃ for 12 hours in a graphite digestion instrument.
(4) Taking down, cooling to room temperature, and directly metering to 50 mL.
(5) Preparing a standard working solution containing 19 elements of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc, setting the working conditions of a spectrometer instrument, selecting spectral line wavelengths of the elements, and drawing a standard curve by using an inductively coupled plasma emission spectrometer.
(6) Introducing the test solution obtained in the step (4) (filtered by rapid filter paper if necessary) into an inductively coupled plasma emission spectrometer, and performing machine-based determination on the contents of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc in the test solution by using a peak area determination method.
Results and analysis
5.1 Linear Range and correlation coefficient, correlation data as follows:
| element(s) | Linear Range (mg/L) | Correlation coefficient |
| Lead (II) | 0.10-0.50 | 0.999045 |
| Cadmium (Cd) | 0.10-0.50 | 0.999942 |
| Chromium (III) | 0.10-0.50 | 0.999862 |
| Aluminium | 1.00-10.0 | 0.999550 |
| Boron | 2.00-10.0 | 0.999900 |
| Barium salt | 0.20-1.00 | 0.999951 |
| Calcium carbonate | 20.0-100 | 0.999486 |
| Copper (Cu) | 0.20-1.0 | 0.999249 |
| Iron | 0.10-0.50 | 0.999520 |
| Potassium salt | 20.0-100 | 0.999963 |
| Magnesium alloy | 2.00-10.0 | 0.999769 |
| Manganese oxide | 0.20-1.00 | 0.999863 |
| Sodium salt | 20.0-100 | 0.999798 |
| Nickel (II) | 0.10-0.50 | 0.999805 |
| Phosphorus (P) | 20.0-100 | 0.999700 |
| Strontium salt | 0.20-1.00 | 0.999922 |
| Titanium (IV) | 0.20-1.00 | 0.999146 |
| Vanadium oxide | 0.20-1.00 | 0.999854 |
| Zinc | 0.10-0.50 | 0.998525 |
The barium, strontium, titanium, copper, manganese and vanadium have good linearity within the concentration range of 0.20-1.00 mg/L, and the correlation coefficient is more than 0.999; the calcium, potassium, phosphorus and sodium are good in linearity within the concentration range of 20.0-100 mg/L, and the correlation coefficient is larger than 0.999; the aluminum, magnesium and boron are good in linearity within the concentration range of 2.00-10.0 mg/L, and the correlation coefficient is larger than 0.999; the lead, cadmium, chromium, iron, nickel and zinc have good linearity in the concentration range of 0.10-0.50 mg/L, and the correlation coefficient is more than 0.998.
5.2 recovery test
According to the experimental method, under the optimal experimental condition, different additive quantities are selected according to the linear range and the background value condition, the recovery rate test is carried out, and the result is shown in the following table.
As can be seen from the table above, the recovery rates of the 19 elements by adding the standard are all between 97.3 and 108 percent, the recovery rates are good, and the method can meet the requirements.
5.3 precision test
According to the experimental method, under the optimal experimental conditions, 7 times of parallel experiments of the samples are carried out, and the precision of the method is examined according to the detection value (or the intensity of the response signal), and the results are shown in the following table.
As can be seen from the table above, in the method, the RSD of 19 elements is 0.52-2.04%, the experimental requirement of less than 3% is met, and the precision is good. The precision experiment is reliable.
5.4 detection Limit test
According to the experimental method, under the optimal experimental conditions, 21 blank experiments of the sample are carried out, the standard deviation is measured, 3 times of the standard deviation value is taken as the method detection limit, and the results are shown in the following table.
| Element(s) | Detection limit (mg/L) |
| Lead (II) | 0.081 |
| Cadmium (Cd) | 0.015 |
| Chromium (III) | 0.1 |
| Aluminium | 0.039 |
| Boron | 0.063 |
| Barium salt | 0.003 |
| Calcium carbonate | 1.554 |
| Copper (Cu) | 0.003 |
| Iron | 0.2 |
| Potassium salt | 0.471 |
| Magnesium alloy | 0.006 |
| Manganese oxide | 0.03 |
| Sodium salt | 0.243 |
| Nickel (II) | 0.15 |
| Phosphorus (P) | 0.132 |
| Strontium salt | 0.04 |
| Titanium (IV) | 0.015 |
| Vanadium oxide | 0.009 |
| Zinc | 0.006 |
As can be seen from the data in the above table, the detection limit of the method is low except for 19 elements, and the method has high detection capability. In conclusion, the method has good recovery rate, precision and detection limit, the reliability of the method is proved, and meanwhile, the method has the advantages of being simple in operation, time-saving and labor-saving, wide in application range and worthy of popularization.
6. Example 2
Other steps were the same as in example 1, and several other representative surfactants, sodium dodecylbenzenesulfonate (anionic surfactant), octadecyl (stearic acid) hydrochloride (cationic surfactant), alkyldimethyl betaine (zwitterionic surfactant), and myristic acid, which is representative of oleochemicals, were selected for implementation. The methodology data (primary study recovery and precision data, detection limit data from blank tests, no replicates) obtained are as follows:
as can be seen from the data in the table above, the recovery rate of each element of the three surfactants of sodium dodecyl benzene sulfonate (anionic surfactant), octadecyl (stearic acid) hydrochloride (cationic surfactant) and alkyl dimethyl betaine (zwitterionic surfactant) is between 95.7 and 104.0 percent, the precision is between 0.19 and 1.60 percent, and the methodological data is good; the recovery rate of each element of the myristic acid is 95.1-104.3, the precision is 0.23-2.87%, and the methodological data is good.
7. Conclusion
It can be seen from the combination of example 1 and example 2 that, in the method, four typical surfactants, namely sodium dodecylbenzenesulfonate (anionic surfactant), octadecyl (stearic acid) hydrochloride (cationic surfactant), alkyl dimethyl betaine (zwitterionic surfactant), fatty acid monoglyceride (nonionic surfactant) and myristic acid (grease chemical) all have good recovery rate, precision and detection limit, thus proving the reliability and adaptability of the method, and the method has the advantages of simple operation, time saving and labor saving, and is worthy of popularization.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent alterations and equivalents, which are included in the scope of the present invention.
Claims (6)
1. A method for rapidly detecting 19 elements in a surfactant and an oil chemical comprises the following steps:
1) accurately weighing 0.3-1.0g of uniform sample in a centrifuge tube;
2) adding 3-7mL of nitric acid into the centrifuge tube, covering the centrifuge tube, performing ultrasonic oscillation, then adding 0.2-0.6mL of hydrogen peroxide, covering the centrifuge tube, and screwing tightly;
3) digesting at the temperature of 115 ℃ and 120 ℃ in a digestion instrument;
4) taking down, cooling to room temperature, and directly fixing the volume;
5) preparing a standard working solution containing 19 elements of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc, setting the working conditions of a spectrometer instrument, selecting spectral line wavelengths of the elements, and drawing a standard curve by using an inductively coupled plasma emission spectrometer;
6) and (4) introducing the test solution obtained in the step (4) into an inductively coupled plasma emission spectrometer, and performing on-machine determination on the contents of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc in the test solution by using a peak area determination method.
2. A method for rapidly detecting 19 elements in a surfactant and an oil chemical comprises the following steps:
1) accurately weighing 0.3-1.0g of uniform sample in a centrifuge tube with a screw cap;
2) adding 5mL of nitric acid into the centrifuge tube, covering the centrifuge tube, performing ultrasonic oscillation for 10 minutes, adding 0.4mL of hydrogen peroxide, covering the centrifuge tube, and screwing tightly;
3) digesting for 1.5-2 hours at the temperature of 115 ℃ and 120 ℃ in a graphite digestion instrument;
4) taking down, cooling to room temperature, and directly metering to 50 mL;
5) preparing a standard working solution containing 19 elements of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc, setting the working conditions of a spectrometer instrument, selecting spectral line wavelengths of the elements, and drawing a standard curve by using an inductively coupled plasma emission spectrometer;
6) and (4) introducing the test solution obtained in the step (4) into an inductively coupled plasma emission spectrometer, and performing computer measurement on the contents of lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc in the test solution by using a peak area measurement method.
3. The method for rapidly detecting 19 elements in surfactants and oleochemicals according to claim 2, wherein: the uniform sample in the step 1) comprises 0.3-0.5g of solid sample or 0.5-1.0g of liquid sample.
4. The method for rapidly detecting 19 elements in surfactants and oleochemicals according to claim 3, wherein: the centrifuge tube in the step 1) is a flat-bottom or conical-bottom 50mL polypropylene centrifuge tube.
5. The method for rapidly detecting 19 elements in surfactants and oleochemicals according to claim 4, wherein: and 6) filtering the test solution in the step 6) by using quick filter paper.
6. The method for rapidly detecting 19 elements in surfactants and oleochemicals according to claim 5, wherein: the 19 elements are lead, cadmium, chromium, aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc.
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