KR101349163B1 - A method for quantitative analysis of polycarbonate/acrylonitrile-butadiene-styrene using an elemental analyzer - Google Patents
A method for quantitative analysis of polycarbonate/acrylonitrile-butadiene-styrene using an elemental analyzer Download PDFInfo
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- 239000004417 polycarbonate Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 14
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 13
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 title description 30
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 title description 24
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 title description 24
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims abstract description 29
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 24
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 229910052717 sulfur Inorganic materials 0.000 claims description 16
- 239000002775 capsule Substances 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 238000004817 gas chromatography Methods 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000006479 redox reaction Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052734 helium Inorganic materials 0.000 abstract description 2
- 239000001307 helium Substances 0.000 abstract description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229920007019 PC/ABS Polymers 0.000 abstract 2
- 239000000463 material Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 10
- -1 Polyethylene Polymers 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 4
- 238000011088 calibration curve Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 4
- 238000004566 IR spectroscopy Methods 0.000 description 3
- 238000005481 NMR spectroscopy Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- QZRGKCOWNLSUDK-UHFFFAOYSA-N Iodochlorine Chemical compound ICl QZRGKCOWNLSUDK-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000012994 photoredox catalyst Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000003570 air Substances 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- 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
- G01N33/44—Resins; Plastics; Rubber; Leather
- G01N33/442—Resins; Plastics
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
Description
본 발명은 PC/ABS 블렌드의 함유량 분석 방법에 관한 것으로서, 더욱 상세하게는 자동차의 그릴 및 대시패널 부품 등에 사용하는 PC/ABS 블렌드에서의 주 고분자(BASE POLYMER)인 폴리카보네이트, 아크릴로니트릴, 부타디엔 및 스티렌의 함량을 검량선 작성단계 없이 분석하는 방법에 관한 것이다.
The present invention relates to a method for analyzing the content of PC / ABS blends, and more particularly, polycarbonate, acrylonitrile, butadiene, which is the main polymer (BASE POLYMER) in PC / ABS blends used in automobile grills and dash panel parts. And it relates to a method of analyzing the content of styrene without the calibration curve preparation step.
차량에 적용되고 있는 플라스틱 재료 중에서 ABS (Acrylonitrile-Butadiene-Styrene)계 재료는 폴리올레핀 계 (Polyethylene, Polypropylene) 및 PVC 재료 다음으로 많은 비중을 차지하고 있다. 그러나, 개발초기 도면 재료 사양에 명기되어 있는 재료와 상이한 재료가 적용되고 있는 경우가 빈번하여 물성저하에 따른 품질문제를 일으키는 한 원인이 되고 있는 바, 실제로 제품에 적용되고 있는 PC/ABS 재료의 함량비를 정밀 분석하여 도면 사양과 일치 여부를 확인할 수 있는 방법의 개발이 절실한 실정이다.ABS (Acrylonitrile-Butadiene-Styrene) based on the plastic material used in the vehicle occupies the second largest proportion after the polyolefin (Polyethylene, Polypropylene) and PVC material. However, a material different from the material specified in the drawing material specification at the beginning of development is often applied, which causes a quality problem due to deterioration of physical properties. Therefore, the content of PC / ABS material actually applied to the product It is urgently needed to develop a method for precisely analyzing the ratio and confirming whether it matches the drawing specifications.
고분자 혼합물에 함유된 각 구성 분자의 함유량을 측정하는 종래의 방법으로는, 특허출원 제10-2006-0085314호에서, 열가소성 수지인 폴리프로필렌과 폴리에틸렌 블랜드 소재에서의 폴리프로필렌 함량을 시차주사 열량계를 사용하여 폴리프로필렌의 엔탈피 값을 구하여 산출식에 대입하는 것으로 결정성이 높은 고분자 재료의 정량 분석 방법을 개시하고 있는바, 이는 폴리프로필렌과 폴리에틸렌의 연소시 엔탈피 차이를 이용하는 것이다.As a conventional method for measuring the content of each constituent molecule contained in the polymer mixture, in Patent Application No. 10-2006-0085314, the polypropylene content of the thermoplastic resin and the polyethylene blend material using a differential scanning calorimeter By quantifying the enthalpy value of polypropylene and substituting it into the calculation formula, a method for quantitative analysis of high crystallinity polymer material is disclosed, which uses the enthalpy difference in combustion of polypropylene and polyethylene.
특허출원 제10-2010-0048664호에서는, ABS 수지내의 부타디엔 이중결합을 염화요오드(ICl)를 사용하여 단일결합으로 치환시키고, 남아있는 염화요오드를 요오드화칼륨(KI)와 반응시켜 요오드 이온(I2)를 생성시킨 후, 이를 티오황산나트륨을 사용하여 적정하여 부타디엔의 함량을 분석하는 방법에 관한 것이며, 또한 상기 방법에 의해 부타디엔 함량을 산출하고, ABS 수지 내의 SAN을 용해시켜 제거하여 SAN-그래프트-부타디엔의 양을 측정함으로써 SAN-그래프트-부타디엔 내의 SAN 그래프트율을 분석하는 방법으로서, 크게는 두 단계, 상세하게는 4단계 이상의 과정을 거쳐 구성 분자의 함량을 측정하는 방법을 개시하고 있다.In patent application No. 10-2010-0048664, butadiene double bond in ABS resin is replaced by a single bond using iodine chloride (ICl), and the remaining iodine chloride is reacted with potassium iodide (KI) to make iodine ions (I 2). ), Followed by titration using sodium thiosulfate to analyze the content of butadiene, and also to calculate the butadiene content by the above method, and by dissolving and removing SAN in the ABS resin, SAN-graft-butadiene As a method of analyzing the SAN graft rate in SAN-graft-butadiene by measuring the amount of, it is disclosed a method of measuring the content of the constituent molecules in two steps, in particular four or more steps.
한편, 특허출원 제10-2008-0018752호는 열분해 거동을 이용한 PVC+ABS 블렌드 소재를 TGA를 통하여 각각의 이성분의 함유량을 간단하게 산출할 수 있도록 함으로써, 이성분(예. PC 및 ABS)의 유기물로 이루어진 블렌드 소재의 정량 분석방법을 개시하고 있다. 그러나 상기 어느 발명도 PC/ABS 블렌드의 공중합체가 아닌 각 유기 분자(폴리카보네이트, 아크릴로니트릴, 부타디엔 및 스티렌)의 함량을 정량적으로 분석하는 방법에 대해 개시하고 있지 않다.On the other hand, Patent Application No. 10-2008-0018752 is a PVC + ABS blend material using the pyrolysis behavior to simplify the calculation of the content of each of the two components through the TGA, so that the two components (eg PC and ABS) Disclosed is a quantitative analysis method of a blend material composed of organic materials. However, none of the above inventions discloses a method for quantitatively analyzing the content of each organic molecule (polycarbonate, acrylonitrile, butadiene and styrene) that is not a copolymer of a PC / ABS blend.
한편, PC/ABS의 각 성분별 정량분석을 위해 기존에 사용하는 방법은 적외선 분광기 (Infrared Spectroscopy, IR) 또는 핵자기공명 분광기 (Nuclear Magnetic Resonance spectroscopy, NMR) 을 이용해서 각 성분의 특성 피크 위치 및 형태로부터 성분 종류뿐만 아니라 각 성분별 함량까지 분석하는 것이다. 하지만, 적외선 분광법은 정량분석을 위한 검량선을 얻기 위해 각 성분별 함량을 정확히 알고 있는 PC/ABS 조성비별 표준시료가 필요하기 때문에 표준시료를 구할 수 없는 경우 분석이 불가하다는 단점이 있다. NMR을 사용한 분석법은 검량선이 필요없으므로 표준시료 문제는 없으나 ABS 소재의 특성상 NMR 스펙트럼에 나타나는 신호들간의 중첩이 매우 심해서 정성은 가능하나, 정확한 정량결과를 얻기에는 오차율이 매우 크다는 단점이 있다. 따라서 제조가 곤란한 소재 조성별 표준시료 유무의 제한없이 PC/ABS 수지내 성분별 함량비에 대한 정량 분석을 간편하고 정확하게 할 수 있는 새로운 방법이 요구되고 있는 실정이다.
In the meantime, conventional methods for quantitative analysis of each component of PC / ABS are performed by using infrared spectroscopy (IR) or nuclear magnetic resonance spectroscopy (NMR). It analyzes not only the type but also the content of each component. However, infrared spectroscopy requires a PC / ABS composition ratio standard sample that accurately knows the content of each component to obtain a calibration curve for quantitative analysis. As NMR method does not require calibration curve, there is no standard sample problem. However, due to the nature of ABS material, the overlap between signals appearing in NMR spectrum is very serious, but the error rate is very large to obtain accurate quantitative results. Therefore, there is a need for a new method that can easily and accurately quantitatively analyze the content ratio of each component in the PC / ABS resin without the limitation of having a standard sample for each composition.
본 발명은 PC/ABS 함량별 다수의 표준시료가 필요한 번거로운 검량선 작성 단계를 거치지 않고 직접 PC/ABS 내 각 성분의 함량 분석이 가능한 분석법을 제공하고자 한다.The present invention is to provide an analysis method that can directly analyze the content of each component in the PC / ABS without a cumbersome calibration curve step that requires a number of standard samples for each PC / ABS content.
본 발명은; SUMMARY OF THE INVENTION
a) PC/ABS 시료를 Sn캡슐 및 Ag캡슐에 넣는 단계;a) placing the PC / ABS sample in Sn capsules and Ag capsules;
b) 시료가 반응기 내에서 연소된 후 촉매와 산화 및 환원반응을 거치는 단계;b) undergoing oxidation and reduction with the catalyst after the sample is combusted in the reactor;
c) 상기 단계에서 산화환원반응을 거친 기체를 가스크로마토그래피(GC) 데이터로 분리하여 CO2,H2O,N2,SO2및 CO의 함량비를 얻어 C, H, N, S, O 각 원소의 함량비를 얻는 단계 및c) separating the gas subjected to the redox reaction in the step by gas chromatography (GC) data to obtain a content ratio of CO 2 , H 2 O, N 2 , SO 2 and CO to obtain C, H, N, S, O Obtaining a content ratio of each element; and
d)하기의 수학식 1~8로부터 PC(폴리카보네이트), A(아크릴로니트릴), B(부타디엔) 및 S(스티렌)의 함량비를 얻는 단계를 포함하는 PC/ABS의 성분 정량 분석 방법을 제공한다.d) a method for quantitative analysis of components of PC / ABS comprising the step of obtaining the content ratio of PC (polycarbonate), A (acrylonitrile), B (butadiene) and S (styrene) from Equations 1 to 8 to provide.
본 발명은 PC/ABS 수지의 정량 분석방법에 관한 것으로, 보다 상세하게는 원소분석기(Elemental Analyzer)를 이용하여 PC/ABS 수지의 주성분인 폴리카보네이트, 아크릴로니트릴, 부타디엔 및 스티렌의 함량을 간단하고 정확히 정량할 수 있다. 이러한 PC/ABS 재료의 정확한 정량분석 방법의 정립으로 설계도면 또는 재료스펙에 명시된 재료와는 상이한 조성비의 재료를 적용함으로써 발생하는 자동차 부품의 물성저하에 따른 품질문제의 원인 분석이 가능하다.
The present invention relates to a method for quantitative analysis of a PC / ABS resin, and more particularly, by using an elemental analyzer (Elemental Analyzer), the content of polycarbonate, acrylonitrile, butadiene and styrene, which are the main components of the PC / ABS resin, It can be accurately quantified. By establishing accurate quantitative analysis method of PC / ABS materials, it is possible to analyze the cause of quality problems caused by the deterioration of the physical properties of automobile parts caused by applying materials with composition ratio different from those specified in design drawings or material specifications.
도1은 본 발명의 PC/ABS 수지의 정량 분석방법을 간략하게 도식화한 것으로서, 샘플러, 컬럼등을 포함하는 원소분석기를 포함한다. 본 발명에 사용될 수 있는 원소분석기는 당해 기술분야에서 사용될 수 있는 종류로서 특별히 제한하지 않는다.1 is a schematic diagram illustrating a quantitative analysis method of a PC / ABS resin of the present invention, and includes an elemental analyzer including a sampler, a column, and the like. The elemental analyzer that can be used in the present invention is not particularly limited as a kind that can be used in the art.
PC/ABS를 구성하는 4가지 화합물 PC(Polycarbonate), A(Acrylonitrile), B(Butadiene) 및 S(Styrene)의 화학구조는 다음과 같다.The chemical structures of the four compounds constituting PC / ABS, PC (Polycarbonate), A (Acrylonitrile), B (Butadiene) and S (Styrene) are as follows.
PC: 화학식 C16H14O3, 분자량 254.28
PC: chemical formula C 16 H 14 O 3 , molecular weight 254.28
A: 화학식 C3H3N, 분자량 53.06A: chemical formula C 3 H 3 N, molecular weight 53.06
B: 화학식 C4H6, 분자량 54.09B: chemical formula C 4 H 6 , molecular weight 54.09
S: 화학식 C8H8, 분자량 104.15S: chemical formula C 8 H 8 , molecular weight 104.15
상기 화학식과 분자량 정보로부터, PC,A,B,S가 각기 x,y,z,w 개수로 구성된 PCxAxBySz를 구성하는 원소별 개수 및 함량비는 아래 수학식 1~4로 정리됨을 알 수 있다. (원자량: C 12.01, H 1.01, N 14.01, O 16.00)From the chemical formula and molecular weight information, it can be seen that the number and content ratio of each element constituting PCxAxBySz each consisting of the number of x, y, z, w of PC, A, B, S are summarized by Equations 1 to 4 below. (Atomic Weight: C 12.01, H 1.01, N 14.01, O 16.00)
수학식 1Equation 1
PCxAxBySz 내 C 개수 = 16x + 3y + 4z + 8w Number of C in PCxAxBySz = 16x + 3y + 4z + 8w
C 함량(%) = (192.16x+36.03y+48.04z+96.08w)/SUM*100 C content (%) = (192.16x + 36.03y + 48.04z + 96.08w) / SUM * 100
수학식 2Equation 2
PCxAxBySz 내 H 개수 = 14x + 3y + 6z + 8wH count in PCxAxBySz = 14x + 3y + 6z + 8w
H 함량(%) = (14.14x+3.03y+6.06z+8.08w)/SUM*100 H content (%) = (14.14x + 3.03y + 6.06z + 8.08w) / SUM * 100
수학식 3Equation 3
PCxAxBySz 내 N 개수 = yN counts in PCxAxBySz = y
N 함량(%) = (14.01y)/SUM*100 N content (%) = (14.01y) / SUM * 100
수학식 4Equation 4
PCxAxBySz 내 O 개수 = 3xO count in PCxAxBySz = 3x
O 함량(%) = (48x)/SUM*100 O content (%) = (48x) / SUM * 100
(SUM = 254.3x + 53.34y + 54.64z + 104.16w)(SUM = 254.3x + 53.34y + 54.64z + 104.16w)
C, H, N, O 각 원소의 무게함량을 원소분석기로 측정하여, PC, A, B 및 S의 개수비인 x, y, z, w를 수학식 1 내지 4로부터 계산할 수 있다. PC, A, B 및 S 각각의 개수비와 분자량으로부터 PC, A, B 및 S 함량비는 아래 수학식 5 내지 8로부터 계산할 수 있다.By measuring the weight content of each element of C, H, N, O with an element analyzer, x, y, z, w, which is the number ratio of PC, A, B, and S, can be calculated from Equations 1 to 4. PC, A, B and S content ratio from the number ratio and molecular weight of each of PC, A, B and S can be calculated from Equations 5 to 8 below.
수학식 5Equation 5
PCxAxBySz 내 PC함량(%) = 254.27x /(254.28x + 53.06y + 54.09z + 104.15w)*100PC content in PCxAxBySz (%) = 254.27x / (254.28x + 53.06y + 54.09z + 104.15w) * 100
수학식 6Equation 6
PCxAxBySz 내 A 함량(%) = 53.06y /(254.28x + 53.06y + 54.09z + 104.15w)*100 % A content in PCxAxBySz = 53.06y / (254.28x + 53.06y + 54.09z + 104.15w) * 100
수학식 7Equation 7
PCxAxBySz 내 B 함량(%) = 54.09z /(254.28x + 53.06y + 54.09z + 104.15w)*100 % B content in PCxAxBySz = 54.09z / (254.28x + 53.06y + 54.09z + 104.15w) * 100
수학식 8Equation 8
PCxAxBySz 내 S 함량(%)=104.15w/(254.28x + 53.06y + 54.09z + 104.15w)*100 S content in PCxAxBySz (%) = 104.15w / (254.28x + 53.06y + 54.09z + 104.15w) * 100
본 발명은; SUMMARY OF THE INVENTION
a) PC/ABS 시료를 Sn캡슐 및 Ag캡슐에 넣는 단계;a) placing the PC / ABS sample in Sn capsules and Ag capsules;
b) 원소 분석기에 수송기체로서 헬륨, 산소 및 공기를 주입하고 온도를 승온하여 시료가 반응기 내에서 연소된 후 촉매와 산화 및 환원반응을 거치는 단계;b) injecting helium, oxygen and air into the elemental analyzer as a transport gas and raising the temperature to undergo oxidation and reduction with the catalyst after the sample is combusted in the reactor;
c) 상기 단계에서 산화환원반응을 거친 기체를 가스크로마토그래피(GC) 데이터로부터 CO2, H2O, N2 및 CO의 함량비를 얻어 C, H, N, O 각 원소의 함량비를 얻는 단계 및c) obtaining a content ratio of CO 2 , H 2 O, N 2 and CO from the gas chromatography (GC) data of the gas subjected to the redox reaction in the above step to obtain the content ratio of each element of C, H, N, O Steps and
d) 측정된 C, H, N, O, S의 함량비와 상기의 수학식 1~8로부터 PC(폴리카보네이트), A(아크릴로니트릴), B(부타디엔) 및 S(스티렌)의 함량비를 얻는 단계를 포함하는 PC/ABS의 성분 정량 분석 방법을 제공한다.d) the content ratio of the measured C, H, N, O, S and the content ratio of PC (polycarbonate), A (acrylonitrile), B (butadiene) and S (styrene) from Equations 1 to 8 It provides a method for quantitative analysis of the components of the PC / ABS comprising the step of obtaining.
본 발명의 일 구체예를 하기에 더욱 상세하게 설명하고자 하나, 본 발명의 보호받고자 보호받고자 하는 범위가 이에 한정되는 것은 아님을 주지해야 할 것이다.One embodiment of the present invention will be described in more detail below, but it should be noted that the scope of protection of the present invention is not limited thereto.
본 발명은; SUMMARY OF THE INVENTION
a) PC/ABS 시료를 측정원소 종류에 따라 Sn캡슐 (C,H,N,S분석) 및 Ag캡슐(O 분석)에 넣는 단계;a) putting the PC / ABS sample into the Sn capsule (C, H, N, S analysis) and Ag capsule (O analysis) according to the type of the measurement element;
b) 시료가 반응기 내에서 연소된 후 촉매와 산화 및 환원반응을 거치는 단계b) after the sample has been combusted in the reactor, undergoing oxidation and reduction with the catalyst
c) 상기 단계에서 산화환원반응을 거친 기체를 가스크로마토그래피(GC) 데이터로 분리하여 CO2,H2O,N2,SO2및 CO의 함량비를 얻어 C, H, N, S, O 각 원소의 함량비를 얻는 단계 및c) separating the gas subjected to the redox reaction in the step by gas chromatography (GC) data to obtain a content ratio of CO 2 , H 2 O, N 2 , SO 2 and CO to obtain C, H, N, S, O Obtaining a content ratio of each element; and
d) 측정된 C, H, N, O, S의 함량비와 상기의 수학식 1~8로부터 PC(폴리카보네이트), A(아크릴로니트릴), B(부타디엔) 및 S(스티렌)의 함량비를 얻는 단계를 포함하는 PC/ABS의 성분 정량 분석 방법을 제공한다.d) the content ratio of the measured C, H, N, O, S and the content ratio of PC (polycarbonate), A (acrylonitrile), B (butadiene) and S (styrene) from Equations 1 to 8 It provides a method for quantitative analysis of the components of the PC / ABS comprising the step of obtaining.
상기 단계 a)에서 Sn캡슐 및 Ag캡슐에 넣는 PC/ABS 시료는 바람직하게는 1~100 mg로 넣을 수 있으며, 중량 측정시 정확도는 ㎍단위로 측정하는 것이 바람직하다. C,H,N, 및 S의 함량비를 측정할 경우는 Sn캡슐을 사용하며, O의 함량비를 측정할 경우에는 Ag캡슐를 사용한다.The PC / ABS sample in the Sn capsule and Ag capsule in step a) is preferably in the amount of 1 ~ 100 mg, the weight is preferably measured in μg accuracy. Sn capsules are used to measure the content ratio of C, H, N, and S, and Ag capsules are used to measure the content ratio of O.
상기 b)단계에서 온도는 900 ~ 1200℃이며, 바람직하게는 C,H,N,S 분석 온도는 약 1000 ℃, O의 분석 온도는 약 1120 ℃ 이다.In step b), the temperature is 900 to 1200 ° C. Preferably, the analysis temperature of C, H, N, and S is about 1000 ° C and the analysis temperature of O is about 1120 ° C.
상기 c)단계의 가스 크로마토그래피는 통상적으로 이용가능한 CO2,H2O,N2,SO2,CO가 분리가능한 컬럼 이용할 수 있다. Gas chromatography of step c) can be used is a column capable of separating the commonly available CO 2 , H 2 O, N 2 , SO 2 , CO.
상기 d)단계에서 얻어지는 PC(폴리카보네이트), A(아크릴로니트릴), B(부타디엔) 및 S(스티렌)의 함량비는 수학식 1 내지 8을 이용하여 계산할 수 있다. The content ratio of PC (polycarbonate), A (acrylonitrile), B (butadiene) and S (styrene) obtained in step d) may be calculated using Equations 1 to 8.
이하 본 발명의 실시예를 하기에 설명하고자 하나 본 발명의 범위가 이에 한정되는 것은 아님을 주지해야할 것이다.Hereinafter, the embodiments of the present invention will be described below, but it should be noted that the scope of the present invention is not limited thereto.
실시예 1Example 1
표준시료 1 (PC: 65 wt%, A: 5 wt%, B: 10 wt%, S: 20 wt%)Sample 1 (PC: 65 wt%, A: 5 wt%, B: 10 wt%, S: 20 wt%)
표준시료 1을 본 발명의 C,H,N,S 측정시 Sn캡슐에 10 mg 및 O 측정시 Ag캡슐에 10 mg 을 넣고, 반응기온도를 각기 1000, 1120 ℃로 설정하여 열분해 시킨 후 촉매내에서 산화 환원 반응이 모두 진행된 후 GC의 데이터로부터 산출된 C, H, N, O 함량비를 수학식 1~8 에 입력하여 결과를 산출하여 하기 표1에 나타내었다.Standard sample 1 was put in 10 mg in Sn capsules when measuring C, H, N, and S in the present invention, and 10 mg in Ag capsules when measuring O, and pyrolyzed by setting the reactor temperature at 1000 and 1120 ° C., respectively, in the catalyst. After all the redox reactions proceeded, the C, H, N, and O content ratios calculated from the data of GC were entered in Equations 1 to 8, and the results are shown in Table 1 below.
실시예 2Example 2
상기 실시예 1와 동일하게 수행하되, 표준시료 2((PC: 78 wt%, A: 4 wt%, B: 10 wt%, S: 8 wt%)를 이용하여 수행하였다.The same procedure as in Example 1 was carried out using Standard Sample 2 ((PC: 78 wt%, A: 4 wt%, B: 10 wt%, S: 8 wt%).
실시예 3Example 3
상기 실시예 1와 동일하게 수행하되, 표준시료 3((PC: 74 wt%, A: 5 wt%, B: 9 wt%, S: 12 wt%)를 이용하여 수행하였다.The same procedure as in Example 1 was carried out using Standard Sample 3 ((PC: 74 wt%, A: 5 wt%, B: 9 wt%, S: 12 wt%).
표준시료의 조성비와 본 발명의 원소분석 결과에 의한 함량비 분석결과가 잘 일치함을 알 수 있다.
It can be seen that the composition ratio of the standard sample and the content ratio analysis result by the elemental analysis result of the present invention are in good agreement.
PC는 Polycarbonate, A는 Acrylonitrile, B는 Butadiene 및 S는 Styrene이다. PC is Polycarbonate, A is Acrylonitrile, B is Butadiene and S is Styrene.
Claims (1)
b) 시료가 반응기 내에서 연소된 후 촉매와 산화 및 환원반응을 거치는 단계;
c) 상기 단계에서 산화환원반응을 거친 기체를 가스크로마토그래피(GC) 데이터로 분리하여 CO2,H2O,N2,SO2및 CO의 함량비를 얻어 C, H, N, S, O 각 원소의 함량비를 얻는 단계 및
d)하기의 수학식 1~8로부터 PC(폴리카보네이트), A(아크릴로니트릴), B(부타디엔) 및 S(스티렌)의 함량비를 얻는 단계를 포함하는 PC/ABS의 성분 정량 분석 방법.
수학식 1
PCxAxBySz 내 C 개수 = 16x + 3y + 4z + 8w
C 함량(%) = (192.16x+36.03y+48.04z+96.08w)/SUM*100
수학식 2
PCxAxBySz 내 H 개수 = 14x + 3y + 6z + 8w
H 함량(%) = (14.14x+3.03y+6.06z+8.08w)/SUM*100
수학식 3
PCxAxBySz 내 N 개수 = y
N 함량(%) = (14.01y)/SUM*100
수학식 4
PCxAxBySz 내 O 개수 = 3x
O 함량(%) = (48x)/SUM*100
(SUM = 254.3x + 53.34y + 54.64z + 104.16w)
수학식 5
PCxAxBySz 내 PC함량(%) = 254.27x /(254.28x + 53.06y + 54.09z + 104.15w)*100
수학식 6
PCxAxBySz 내 A 함량(%) = 53.06y /(254.28x + 53.06y + 54.09z + 104.15w)*100
수학식 7
PCxAxBySz 내 B 함량(%) = 54.09z /(254.28x + 53.06y + 54.09z + 104.15w)*100
수학식 8
PCxAxBySz 내 S 함량(%)=104.15w/(254.28x + 53.06y + 54.09z + 104.15w)*100
(x,y,z,w 는 PC/ABS시료 내 각기 PC(Polycarbonate),A(Acrylonitrile), B(Butadiene) 및 S(Styrene)의 개수를 나타낸다.)
a) placing the PC / ABS sample in Sn capsules and Ag capsules;
b) undergoing oxidation and reduction with the catalyst after the sample is combusted in the reactor;
c) separating the gas subjected to the redox reaction in the step by gas chromatography (GC) data to obtain a content ratio of CO 2 , H 2 O, N 2 , SO 2 and CO to obtain C, H, N, S, O Obtaining a content ratio of each element; and
d) Method of quantitative analysis of PC / ABS comprising the step of obtaining the content ratio of PC (polycarbonate), A (acrylonitrile), B (butadiene) and S (styrene) from the following equations (1) to (8).
Equation 1
Number of C in PCxAxBySz = 16x + 3y + 4z + 8w
C content (%) = (192.16x + 36.03y + 48.04z + 96.08w) / SUM * 100
Equation 2
H count in PCxAxBySz = 14x + 3y + 6z + 8w
H content (%) = (14.14x + 3.03y + 6.06z + 8.08w) / SUM * 100
Equation 3
N counts in PCxAxBySz = y
N content (%) = (14.01y) / SUM * 100
Equation 4
O count in PCxAxBySz = 3x
O content (%) = (48x) / SUM * 100
(SUM = 254.3x + 53.34y + 54.64z + 104.16w)
Equation 5
PC content in PCxAxBySz (%) = 254.27x / (254.28x + 53.06y + 54.09z + 104.15w) * 100
Equation 6
% A content in PCxAxBySz = 53.06y / (254.28x + 53.06y + 54.09z + 104.15w) * 100
Equation 7
% B content in PCxAxBySz = 54.09z / (254.28x + 53.06y + 54.09z + 104.15w) * 100
Equation 8
S content in PCxAxBySz (%) = 104.15w / (254.28x + 53.06y + 54.09z + 104.15w) * 100
(x, y, z, w represents the number of PC (Polycarbonate), A (Acrylonitrile), B (Butadiene) and S (Styrene) in PC / ABS samples, respectively.)
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| KR20110129181A (en) * | 2010-05-25 | 2011-12-01 | 현대자동차주식회사 | Quantitative analysis method of acrylonitrile butadiene styrene copolymer for rubber contents and grafting ratio |
| KR101113645B1 (en) | 2010-07-27 | 2012-02-14 | 현대자동차주식회사 | Quantitative analysis method of Acrylonitrile and Additive in Acrylonitrile-Butadiene rubber composition |
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| KR20040026868A (en) * | 2002-09-26 | 2004-04-01 | 현대자동차주식회사 | Method for Quantitative Analysis of ABS resin |
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