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, abbreviation PAEs, formed phthalic acid esters. Mainly used as plasticizer, resin, caoutchouc, etc can become even more 薬 soft, are often added in ethylene oxide these common material, donc, phthalic acid ester material widely exists in the toys, food packaging materials, medical patient and hose, huile de graissage, a products, electronic products such as hundreds of products.
Because of phthalic acid esters material has stronger metastatic, from long-term exposure to plastic products, food packaging on food or unload into the skin, to enter the body, this kind of material in the human body plays a role similar to estrogen, may interfere with the endocrine, endanger human body health. Various countries have issued standards of phthalic acid esters substances in food contact materials, children’s toys, produits de beauté, etc.. The usage of articles for daily use is limited.
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
In recent years, the eu has been closely watched compulsory standards – “about limit use of certain harmful components in electrical and electronic equipment directive RoHS directive, relative to the old version, how will the new European RoHS directive called RoHS2.0), In the promulgation of the latest version will also be phthalate (2 – ethyl) ester (DEHP), butyl phthalate (DBP), phthalic acid butyl benzyl ester and phthalate (BBP) butyl ester (DIBP), these four substances added to limit the use of the material. 0.1% of these substances with homogeneous material 6 as the maximum allowable concentration, on July 22, 2019. Since the implementation of the directive in EU listed all of the electrical and electronic equipment (except for medical devices and monitoring control) and its downstream suppliers such as production of spare parts, raw materials and packaging are all involve the DEHP, DBP and BBP, DIBP content detection.
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) méthode, 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) méthode “, 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
acetonitrile
The color of pure
2
Ethyl acetate
Analysis of pure
3
Deionized water
18.2MΩ
4
BBP、DIBP、DBP、DEHP
≤99%
Tableau 1-3 main sample preparation equipment
The serial number
The name of the
specifications
note
1
Solvent filter
1000mL
Mobile phase filtration
2
Diaphragm vacuum pump
0.08MPa,160W
Mobile phase filtration, GM-0.33UN
3
Balance analytique
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, etc.
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
Chromatographic column: Elite RoHS phthalates analysis special column
Mobile phase: UN: acetonitrile (1%), B: water (gradient elution)
Traffic: 2.0 mLmin
detection wavelength 225 nm
Taille de l'échantillon: 20 mu L
Column temperature:35 ℃
1.4
The experimental results,
1.4.1
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
linear
ugml mixture concentration, respectively, 10 ug/mL, 20 ugml, 50 ug/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 and BBP, DIBP in 1 ugml – 100 ug/mL concentration range, good linear correlation.
Chromatographic column: Elite RoHS phthalates analysis special column
Mobile phase: UN: acetonitrile (1%), Bwater (gradient elution)
Traffic: 2.0 mL/min
detection wavelength: 225 nm
Taille de l'échantillon: 20 mu L
Column temperature 35 ℃
The concentration of 20 ug/mL four phthalic
Acid ester liquid is injected into high performance liquid chromatograph
RoHS 2.0 Instruction Analytical Test Solution -LC3000 Liquid Chromatograph
Detection limit and the quantitative limit
To three times the signal-to-noise ratio corresponds to the concentration of detection limit, 10 times the signal-to-noise ratio corresponds to the concentration of quantitative restrictions, 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, haute sensibilité, satisfy RoHS2.0 instruction of DEHP,DBP and BBP, DIBP limit concentration detection requirements