CS240470B1 - Method of monomer and diluent residues determination in solid lignocellulose materials - Google Patents
Method of monomer and diluent residues determination in solid lignocellulose materials Download PDFInfo
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- CS240470B1 CS240470B1 CS844457A CS445784A CS240470B1 CS 240470 B1 CS240470 B1 CS 240470B1 CS 844457 A CS844457 A CS 844457A CS 445784 A CS445784 A CS 445784A CS 240470 B1 CS240470 B1 CS 240470B1
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- determination
- formaldehyde
- diluents
- sample
- monomer
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- 239000000178 monomer Substances 0.000 title claims abstract description 21
- 239000003085 diluting agent Substances 0.000 title claims abstract description 13
- 239000007787 solid Substances 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title claims description 17
- 239000000463 material Substances 0.000 title description 17
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000012978 lignocellulosic material Substances 0.000 claims abstract description 6
- 238000004817 gas chromatography Methods 0.000 claims abstract description 4
- 238000004448 titration Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002562 thickening agent Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 63
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000002023 wood Substances 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000011093 chipboard Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000011120 plywood Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- LDKDGDIWEUUXSH-UHFFFAOYSA-N Thymophthalein Chemical compound C1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3C(=O)O2)C=2C(=CC(O)=C(C(C)C)C=2)C)=C1C LDKDGDIWEUUXSH-UHFFFAOYSA-N 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000007799 cork Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- PUFGCEQWYLJYNJ-UHFFFAOYSA-N didodecyl benzene-1,2-dicarboxylate Chemical compound CCCCCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCCCCC PUFGCEQWYLJYNJ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000002025 wood fiber Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Účelom vynálezu je stanovenie zbytkových monomérov a riedidiel v pevných ligstatou riešenia je to, že vzorka z pevného lignocelulózového materiálu sa deštruuje , napr. pomletím, postrúhaním alebo obrúsením pod hladinou rozpúšťadla, ktoré uvolněné zbytkové mdnoméry a riedidlá rozpustí. V získanom roztoku sa koncentrácia určenej látky zistí metodou plynovej chromatografie, spektrofotometricky alebo titračne.The purpose of the invention is to determine residual monomers and diluents in solid ligstat The solution is that the sample from the solid lignocellulosic material is destroyed, e.g. grinding, grinding or abrading below the level of solvent that is released residual thickeners and diluents dissolve. In the obtained solution, the concentration is determined substances are detected by gas chromatography, spectrophotometrically or titrimetrically.
Description
Vynález rieši sposob stanovenia zbytkových monomérov a riedidiel v pevných lignocelulízových materiáloch.The present invention provides a method for determining residual monomers and diluents in solid lignocellulosic materials.
Sňčasný stav stanovenia prchavých látok, tzv. zbytkových monomérov a riedidiel, ako· sú napr. styrén, metylmetakrylát, acetón, etanol, atd'. z drevoplastických materiálov je založený na nepriamej metóde sledovania změny niektorej fyzikálno-mechanickej vlastnosti, napr. tvrdosti, v závislosti na množstve zbytkového monoméru v drevoplastickom materiáli. Rastom množstva zbytkového monoméru klesá tvrdost drevoplastického materiálu. Nevýhodou metody stanovenia tvrdosti materiálu je, že dává len hrubý obraz o množstve nezreagovaného, monoméru v drevoplastickom materiáli. Množstvo rozpúšťadiel v drevoplastickom materiáli sa stanoví zistením hmotnostného úbytku drevoplastického materiálu počas dlhodobého odparovania do· konstantně] hmotnosti.The current state of determination of volatile substances residual monomers and diluents, such as e.g. styrene, methyl methacrylate, acetone, ethanol, etc. of wood-based materials is based on an indirect method of monitoring the change in some physico-mechanical property, e.g. hardness, depending on the amount of residual monomer in the wood-plastic material. Increasing the amount of residual monomer decreases the hardness of the wood-plastic material. A disadvantage of the method of determining the hardness of a material is that it only gives a rough picture of the amount of unreacted monomer in the wood-plastic material. The amount of solvents in the wood-plastic material is determined by determining the weight loss of the wood-plastic material during long-term evaporation to a constant weight.
V dřevných materiáloch, ako sú drevotrieskové došky, dřevovláknité došky, preglejky, korové došky a pod., kde sa používá lepidlo na báze formaldehydu, je potřebné presne stanovit množstvo nezreagovaného formaldehydu v drevnom materiáli. Uvolňujúci sa formaldehyd, podobné ako zbytkové monoméry a rozpúšťadlá popísané v predchádzajúcom případe majú nepriaznivý dopad na hygienu prostredia. Súčasný sposob stanovenia formaldehydu používaný v drevárskych podnikoch, najma v NSR, Rakúsku, Finsku, Taliansku je metódou Fesyp. Popísaná metoda spočívá v extrakcii teliesok o rozmere 25 x 25 x 18 mm toluénom, za teploty varu toluénu počas dvoch hodin.In wood materials such as chipboard, wood fiber, plywood, cork, etc., where a formaldehyde-based adhesive is used, it is necessary to accurately determine the amount of unreacted formaldehyde in the wood material. The release of formaldehyde, similar to the residual monomers and solvents described in the previous case, has an adverse impact on environmental hygiene. The current formaldehyde method used in timber companies, in particular in Germany, Austria, Finland, Italy is the Fesyp method. The described method consists of extracting the bodies of 25 x 25 x 18 mm with toluene at the boiling point of toluene for two hours.
Množstvo formaldehydu sa stanoví titračne z vodného roztoku. Mohl H. R., Holz alš Roh — und Werkstoff, 36, 1978. Podía čs. noriem sa stanoví formaldehyd odpařováním formaldehydu z dezintegrovaného materiálu pri teplote 60 °C počas štyroch hodin nad hladinou vody. Následné sa titračne stanoví množstvo pohlteného formaldehydu vo vodnom roztoku, ktorý bol jednu hodinu chladený v chladničke. Je známy rad dalších metód v hoře uvedenej literatúre, ktoré stanovujú formaldehyd vo vzduchu z okolia vzorky chemickou reakciou formaldehydu s chemickým činidlom- ako pri titračnom stanovení, tak i pri spektrálnom vyhodnotení . Nevýhodou popísaných metód je dlhá doba stanovenia, čo znemožňuje priebežnú kontrolu formaldehydu v technologickom procese a prípadnú úpravu technologických parametrov. Pre urýchlenie uvedených metód sa vo váčšine prípadov používá zvýšená teplota stanovenia. V niektorých prípadoch má zvýšenie teploty nepriaznivý účinok na přesnost stanovenia obsahu formaldehydu. Napr. pri stanovení volného formaldehydu v drevotrieskových doškách metódou Fesyp sa extrakciou vzorky toluénom pri teplote 110,6 °C posúva rovnovážná reakcia medzi formaldehydom a polymérnym paraformaldehydom na stranu monomérneho formaldehydu, Walker J. F., Formaldehyde, Second edition, New York, 1953, čo má za následok stanovenie vyšších hodnot formaldehydu vo vzorke.The amount of formaldehyde is determined by titration from an aqueous solution. Mohl HR, Holz als Roh- und Werkstoff, 36, 1978. The standard is determined by formaldehyde evaporation of formaldehyde from the disintegrated material at 60 ° C for four hours above the water level. Subsequently, the amount of formaldehyde absorbed in the aqueous solution which was cooled in the refrigerator for one hour was determined by titration. A number of other methods are known in the above literature to determine formaldehyde in ambient air from a sample by chemical reaction of formaldehyde with a chemical reagent - both in titration and spectral evaluation. The disadvantage of the described methods is the long determination time, which makes it impossible to continuously check formaldehyde in the technological process and any adjustment of technological parameters. In most cases, an elevated assay temperature is used to accelerate these methods. In some cases, the temperature increase has an adverse effect on the accuracy of the formaldehyde content determination. E.g. in the determination of free formaldehyde in chipboard using the Fesyp method, extraction of the sample with toluene at 110.6 ° C shifts the equilibrium reaction between formaldehyde and polymeric paraformaldehyde to the monomeric formaldehyde side, Walker JF, Formaldehyde, Second Edition, New York, 1953 determination of higher formaldehyde values in the sample.
Uvedené nevýhody súčasného stavu do značnej miery odstraňuje sposob stanovenia zbytkových monomérov a riedidiel v pevných lignocelulózových materiáloch podlá vynálezu, ktorého podstatou je to·, že vzorka pevného lignocelulózového· materiálu sa deštruuje pod hladinou rozpúšfadla a uvolněné zbytkové monoméry a riedidlá sa rozpustia pod hladinou rozpúšfadla a následné sa určí koncentrácia zbytkových monomérov a riedidiel, s výhodou plynovou chromatografiou, spektrofotometricky alebo titračne. 1 The above-mentioned disadvantages of the present state are largely eliminated by the method of determining residual monomers and diluents in the solid lignocellulosic materials according to the invention, which is based on the fact that a sample of solid lignocellulosic material is destroyed below solvent level and released residual monomers and diluents dissolve and the concentration of residual monomers and diluents is subsequently determined, preferably by gas chromatography, spectrophotometrically or by titration. 1
Výhody vynálezu spočívajú v možnosti prlameho stanovenia přesného· obsahu zbytkových monomérov, resp. rozpúšťadiel v drevoplastickom materiáli. V súčasnosti nie je známa metoda na priame a přesné stanovenie zbytkových monomérov, resp. rozpúšťadiel v drevoplastickom materiáli. SpQsobom podfa vynálezu je možné s výhodou využit časovo nenáročné stanovenie formaldehydu v drevnom materiáli na jeho sledovanie počas technologickej přípravy. Spósobom podfa vynálezu sa skráti příprava vzorky pre analytické stanovenie formaldehydu o· 2 až 4 hodiny.The advantages of the invention lie in the possibility of directly determining the exact content of residual monomers and / or residual monomers. solvents in the wood-plastic material. There is currently no known method for the direct and accurate determination of residual monomers, respectively. solvents in the wood-plastic material. According to the invention, it is advantageously possible to use a time-saving determination of formaldehyde in the wood material for its monitoring during technological preparation. The method of the invention shortens sample preparation for the analytical determination of formaldehyde by 2 to 4 hours.
PřikladlEXAMPLE
Vzorka drevoplastického materiálu sa upraví ná rozměr 10 x 10 x 200 mm. Do strúhacieho zariadenia sa naleje presne 100 ml metylalkoholu, zaridenie sa uzavrie a cez otvor sa vzorka ponoří do metylalkoholu. Následné sa vzorka skráti pod hladinou metylalkoholu strúhaním konca vzorky šnekovým nožom. Získané piliny majú rozměr v 93 % v rozmedzí 0,2 až 0,7 mm, zvyšných 7 % má rozměr menší ako· 0,2 milimetrov.The sample of the wood material is adjusted to a size of 10 x 10 x 200 mm. Pour exactly 100 ml of methanol into the grater, close the apparatus and immerse the sample in methanol through the orifice. Subsequently, the sample is shortened below the methyl alcohol level by grating the end of the sample with a screw knife. The sawdust obtained has a dimension of 93% in the range of 0.2 to 0.7 mm, the remaining 7% having a dimension of less than 0.2 mm.
Po 15 minútach sa suspenzia premieša a přefiltruje. Vo filtráte sa stanovia množstvá zbytkových monomérov metylmetakrylátu a styrénu, metódou plynovej chromatografie na koloně dlhej tri metre plnenej Chromosorb W AW — DMCS o zrnitosti 0,14 až 0,15 mm so zakotvenou fázou 15 % didodecylftalátu.After 15 minutes, the suspension is stirred and filtered. Quantities of residual methyl methacrylate and styrene monomers are determined in the filtrate by a gas chromatographic method on a three meter long column packed with Chromosorb W AW - DMCS with a particle size of 0.14 to 0.15 mm with an anchored phase of 15% didodecyl phthalate.
P r í k 1 a d 2Example 1 a d 2
Vzorka drevoplastického materiálu sa spracuje podía příkladu 1 tak, že vo filtráte sa stanoví acetón plynovou chromatografiou za tých istých podmienok ako v příklade 1. Acetón sa použije ako· riedidlo do použitej impregnačnej sústavy.A sample of the wood-plastic material was treated according to Example 1 by determining acetone in the filtrate by gas chromatography under the same conditions as in Example 1. Acetone was used as a diluent to the impregnation system used.
Příklad 3Example 3
Vzorka drevotrieskové]' došky sa spracuje ako v příklade 1 tak, že namiesto metylalkoholu sa použije destilovaná voda. Vo filtráte sa stanoví množstvo formaldehydu po přidaní acetylacetónovej reagencie v poměre 1 : 1 meraním Pulfrichovým spektrofotometrem pri 420 nm. (Mohl H. R.,j.A chipboard sample is treated as in Example 1 by using distilled water instead of methanol. The amount of formaldehyde in the filtrate was determined by adding 1: 1 acetylacetone reagent by Pulfrich spectrophotometer at 420 nm. (Mohl H.R.
P r í k 1 a d 4Example 1 4
Vzorka preglejky sa spracuje ako v příklade 1 tak, že namiesto metylalkoholu sa použije destilovaná voda. V získanom filtráte sa stanoví množstvo volného formaldehydu přidáním indikátora thymolftalein sA plywood sample was treated as in Example 1 by using distilled water instead of methanol. The amount of free formaldehyde in the filtrate obtained is determined by adding the thymolphthalein s indicator
a zneutralizovaním vzorky z 0,05 N hydroxidu sodného do prvého modrého zafarbenia. Vzorka sa ponechá stať 2 minúty, aby reakcia prebehla dokonale. Vytvořený hydroxid sodný sa titruje kyselinou chlorovodíkovou do odfarbenia.and neutralizing the sample from 0.05 N sodium hydroxide to the first blue color. The sample is allowed to stand for 2 minutes to complete the reaction. The sodium hydroxide formed is titrated with hydrochloric acid until discolouration.
Sposob stanovenia zbytkových monoméroy a riedidiel podlá vynálezu sa može uplátnif pri stanovovaní volného formaldehydu v dřevotřískových doškách a v ostatných výrobkoch dřevařského priemyslu, kde sa ako súčasť lepidla použije formaldehyd alebo iné prchavé zdraviu škodlivé látky. V oblasti použitia drevoplastických materiálov je možné stanovit zbytkové monoméry alebo rozpúšťadlá.The method of determining residual monomers and diluents according to the invention can be applied to the determination of free formaldehyde in chipboard and other woodworking products where formaldehyde or other volatile health-damaging substances are used as part of the adhesive. Residual monomers or solvents can be determined in the field of use of wood-plastic materials.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS844457A CS240470B1 (en) | 1984-06-13 | 1984-06-13 | Method of monomer and diluent residues determination in solid lignocellulose materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS844457A CS240470B1 (en) | 1984-06-13 | 1984-06-13 | Method of monomer and diluent residues determination in solid lignocellulose materials |
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| Publication Number | Publication Date |
|---|---|
| CS445784A1 CS445784A1 (en) | 1985-07-16 |
| CS240470B1 true CS240470B1 (en) | 1986-02-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS844457A CS240470B1 (en) | 1984-06-13 | 1984-06-13 | Method of monomer and diluent residues determination in solid lignocellulose materials |
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| CS (1) | CS240470B1 (en) |
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1984
- 1984-06-13 CS CS844457A patent/CS240470B1/en unknown
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| Publication number | Publication date |
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| CS445784A1 (en) | 1985-07-16 |
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