RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
Chapter 1 Determination of four phthalates content
1.1 Foreword
Phthalic acid ester, also called phthalate, afkorting PAE's, formed phthalic acid esters. Mainly used as plasticizer, hars, rubber, etc can become even more 薬 soft, are often added in ethylene oxide these common material, daarom, phthalic acid ester material widely exists in the toys, verpakkingsmateriaal voor voedsel, medical patient and hose, smeerolie, a products, electronic products such as hundreds of products.
Vanwege ftaalzuuresters heeft materiaal sterkere metastatische eigenschappen, van langdurige blootstelling aan plastic producten, voedselverpakking op voedsel of lossen in de huid, to enter the body, this kind of material in the human body plays a role similar to estrogen, kan de hormoonhuishouding verstoren, de gezondheid van het menselijk lichaam in gevaar brengen. Verschillende landen hebben normen uitgevaardigd voor ftaalzuuresters in materialen die met voedsel in contact komen, kinderspeelgoed, cosmetica, enz. Het gebruik van artikelen voor dagelijks gebruik is beperkt.
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
In de afgelopen jaren, de eu heeft de verplichte normen nauwlettend in de gaten gehouden – “about limit use of certain harmful components in electrical and electronic equipment directive RoHS directive, opzichte van de oude versie, hoe zal de nieuwe Europese RoHS-richtlijn RoHS2.0 worden genoemd), In the promulgation of the latest version will also be phthalate (2 – ethyl) ester (DEHP), butylftalaat (DBP), ftaalzuurbutylbenzylester en ftalaat (BBP) butylester (DIBP), deze vier stoffen zijn toegevoegd om het gebruik van het materiaal te beperken. 0.1% of these substances with homogeneous material 6 as the maximum allowable concentration, on July 22, 2019. Sinds de implementatie van de richtlijn in de EU zijn alle elektrische en elektronische apparatuur vermeld (met uitzondering van medische hulpmiddelen en monitoringcontrole) en zijn downstream-leveranciers, zoals de productie van reserveonderdelen, grondstoffen en verpakkingen zijn allemaal betrokken bij DEHP, DBP en BBP, DIBP-inhoudsdetectie.
In December 2019 group standards promulgated by the China electronics standardization technology association of the 1063-2019 – T/CESA electronic electrical products for determination of the four phthalates in high performance liquid chromatography (HPLC) method, and provides for electronic electrical products of four kinds of phthalic acid esters content in high performance liquid chromatographic method, with IEC62321 instrument Determination of electronic products in the restricted substances part 8, 1063-2019 – T/CESA electronic electrical products for determination of the four phthalates in high performance liquid chromatography (HPLC) method “, GB/T28599-2020 “cosmetics in the determination of phthalates material, and literature, puts forward the DEHP, DBP, BBP, DIBP simultaneous determination of four kinds of phthalic acid ester solution, for your reference.
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
Main chemical reagents, standard list serial
number
reagent
The purity
1
acetonitril
The color of pure
2
Ethyl acetate
Analysis of pure
3
Deionized water
18.2MΩ
4
BBP、DIBP、DBP、DEHP
≤99%
Tafel 1-3 main sample preparation equipment
The serial number
The name of the
specificaties
opmerking
1
Solvent filter
1000mL
Mobile phase filtration
2
Diaphragm vacuum pump
0.08MPa,160W
Mobile phase filtration, GM-0.33A
3
Analytical balance
Accurate to 0.0001 G
4
Ultrasonic cleaners
3L/ 6 L,40/60KHz,120 W
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
Mobile phase degassing, AS3120
Other glassware experiments include volumetric flask (1 ml and 5 ml, 10 ml, 100 ml), 50 ml tube, pipetting gun (0-1000 – ul, 0-5000 ul) publish or perish, pad fluid head (1 ml and 5 ml), disposable PVC gloves, one-time mouth, 0.45 um PTFE membrane filter, enz
The experimental method
1.3.1
Standard solution preparation
Four kinds of phthalate standard reserve liquid (2000μg/mL) : accurately weigh BBP, DIBP, DBP, DEHP 50mg each, dissolve with acetonitrile and volume to 25mL.
Four kinds of phthalate standard working liquid: The standard working liquid with acetonitrile was prepared with the concentration of 1ugmL, 10ugmL, 20μg/mL, 50μg/mL and 100μg mL respectively.
1.3.2
Sample Pretreatment
1) Cut the sample into small particles with a particle size of about 1mm and below;
2) Weigh the cut sample about 1.0000g (accurate to 0.1mg) and put it into a 50mL tube with a plug;
3) 30mL acetonitrile was added and ultrasonic extraction was carried out for 70mins
4) Cool to room temperature and strain into 100mL bottle;
5) Plug the test tube and residue with acetonitrile for several times, and combine the washing liquid into a 100mL volumetric bottle, and finally fill it with acetonitrile to 100mL;
6) After filtration with filter membrane to be measured.
1.3.3
The chromatographic conditions
Chromatografische kolom: Elite RoHS phthalates analysis special column
Mobile phase: A: acetonitril (1%), B: water (gradiënt elutie)
Verkeer: 2.0 mLmin
detectie golflengte 225 nm
Steekproefgrootte: 20 mijn L
Kolom temperatuur:35 ℃
1.4
The experimental results,
1.4.1
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
lineair
ugml mixture concentration, respectievelijk, 10 en/ml, 20 ugml, 50 en/ml, 10 ug/mL of standard working fluid, according to the concentration from low to highSample to the abscissa denotes the standard concentration, peak area as the ordinate, draw curve and approved. , in accordance with the solution provided by the instrument and testing methods were analyzed, and the concentration of DEHP, DBP en BBP, DIBP in 1 ugml – 100 ug/mL concentration range, good linear correlation.
Chromatografische kolom: Elite RoHS phthalates analysis special column
Mobile phase: A: acetonitril (1%), Bwater (gradiënt elutie)
Verkeer: 2.0 ml/min
detectie golflengte: 225 nm
Steekproefgrootte: 20 mijn L
Kolom temperatuur 35 ℃
De concentratie van 20 ug/mL four phthalic
Zure estervloeistof wordt geïnjecteerd in hoogwaardige vloeistofchromatograaf
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
Detectielimiet en de kwantitatieve limiet
To three times the signal-to-noise ratio corresponds to the concentration of detection limit, 10 keer komt de signaal-ruisverhouding overeen met de concentratie van kwantitatieve beperkingen, measured detection limit and fixed in the limit of the results are as follows:
the four kinds of phthalic acid lipid of detection limit were lower than Smgkg, hoge gevoeligheid, satisfy RoHS2.0 instruction of DEHP,DBP en BBP, DIBP-limietconcentratiedetectievereisten