Erucamide, determination

Analysts in industry prefer in many cases to maintain consistent methods for their analyses. Recommended ASTM analytical procedures are quite well developed in the rubber and polymer industry. As an example, we mention the standard test method for determination of phenolic antioxidants and erucamide slip additives in LDPE using liquid chromatography [76]. However, the current industry standard test methods (ASTM, AOAC, IUPAC, etc.) use a large number of solvents in vast... 

ASTM D 1996-97, Standard Test Method for Determination of Phenolic Antioxidants and Erucamide Slip Additives in Low Density Polyethylene Using Liquid Chromatography (LC), Annual Book of ASTM Standards, ASTM, West Conshohocken, PA (1997), Vol. 08.01. 

Nonvolatile compounds cannot be analysed unless pyrolysis or derivatisation converts them to a condition amenable to GC. Derivatisation GC (or LC) has been used for several components such as erucamide (imidi-sation for volatility), fatty amines (aromatic amidation for UV detectability), and polyethylene oxides (esterification for both volatility and detectability) [178]. The surface concentration of erucamide on extruded LLDPE films was determined quantitatively by surface washings with ether, followed by evaporation, dissolution... 

Amide waxes like stearamide, oleamide, erucamide are subject to extensive risk assessments under the existing chemicals HPV programme in the USA [169]. The available data indicate that there is no mutagenic or reprotoxic potential identified. Repeated dose feeding studies up to 2 years did not reveal a carcinogenic effect. The NOFL was determined to be >7,500 mg kg body weight/day. 

ASTM D 5815 Standard Test Method for Determination of Phenolic Antioxidants and Erucamide Slip Additives in Linear Low-Density Polyethylene Using Liquid Chromatography This ASTM is very similar to ASTM D 1996, except that LLDPE samples are analyzed, and extraction is performed with either isobutanol or isopropanol prior to liquid-chromatographic separation. Isopropanol is recommended as the extraction solvent for lower crystallinity LLDPE (density 0.925 g/ cm and below), and isobutanol is recommended as the extraction solvent for higher crystallinity LLDPE. As the standard notes, besides Irganox 1010, Irganox 1076, and Isonox 129, the test method should be applicable for the determination of other antioxidants such as Ultranox 626, Ethanox 330, Santanox R, and Topanol CA, but the applicability of this test method has not been investigated for these antioxidants. Precision of the procedure is somewhat poorer compared to that of ASTM D 1996 ... 

ASTM D 6953 Standard Test Method for Determination of Antioxidants and Erucamide Slip Additives in Polyethylene Using Liquid Chromatography This ASTM is technically similar to ASTM D 1996 however, it covers a wider set of procedures. Antioxidants are extracted with either isopropanol (densities less than... 

It is also possible to determine multiadditives in the same sample using FTIR and multivariate analysis methods. For example, the simultaneous determination of the concentrations of silica, erucamide and butylhydroxytoluene in PE were measured using IR spectroscopy and suitable calibration models. The concentrations were between 20 and 1100 wt/ppm (366). A multiadditive method was developed for characterisation of an antiblocking agent (silica) and lubricant (erucamide) in molten low density polyethylene (LDPE) samples (324). 

The feasibility of simultaneous in-line monitoring of additives Irganox 1076, Irgafos 168, Tinuvin 622, erucamide and Armostat 310 is studied in molten LDPE. The near IR (NIR) and UV spectroscopic systems used for the determination of additives are described. Based... 

Multivariate calibration methods were used to establish a new method for measurement of three selected additives in LDPE. The determination of the concentration of silica, erucamide and butylhydroxytoluene was based on IR spectroscopy and a calibration model. The concentrations were between 20 and 1100 wt/ppm. Compared with traditional chemical analyses, the new method was shown to be both time- and cost-effective and to be more precise. The method has potential for quality control of PE. 8 refs. NORWAY SCANDINAVIA WESTERN EUROPE... 

SFE chromatography has also been used in the determination of erucamide and antioxidants in polyethylene (PE) [22], butylated hydroxyl toluene, Isonox 129 and Irganox 1010 in PE [23], and PP [23], antioxidants and UV stabilisers in food packages [24] and secondary antioxidants such as distearyl thiodipropionate and phosphonites in polyolefins [25],... 

D 1996-92 Determination of Phenolic Antioxidants and Erucamide Slip Additives in Low Density Polyethylene Using Liquid Chromatography (LC)... 

PVAc has been determined according to equation Tg = 18.4 - 6.77C + 0.2197C (plasticiser content C in % validity range 0-12.5% correlation coefficient 0.9986) [85]. Whereas further chlorinating (PVCC) increases Tg from approximately 86°C towards 100°C, it can be lowered to almost any value by addition of plasticisers (-40° to +90°C), as indeed is true also for PVAc. When the additive concentration in a resin exceeds a few weight percent, it is often possible to assay the additive calorimetri-cally without extracting it. If the additive is incompatible with the resin, it can be detected in a separate crystalline or glassy phase by either its Tm or Tg and measured quantitatively from A7/f determinations at Tin or Acp measurements at Tg. When an additive is soluble in a polymer, its concentration can be estimated from shifts in Tm or Tg of the resin. Once a master curve of Tg V5. plasticiser concentration has been prepared for a particular PVC composition, it can be used to determine the amount of plasticiser in an unknown formulation of the particular plasticiser, e.g. PVC/DIDP (cfr. Fig. 2.1) [27]. For PVC/DOP a linear relationship from zero to 45 wt.% plasticiser has been reported [86]. DSC was also used in miscibility studies of erucamide and PA 12 [87]. 

ASTM 6953-11 Standard Test Method for Determination of Antioxidants and Erucamide Slip Additives in Polyethylene Using Liquid Chromatograph (LC). 

Bulk-to-surface partitioning of erucamide was determined in linear low density polyethylene, LLDPE, using FTIRmicrospectroscopy. It was confirmed that during processing, the additive is uniformly distributed in... 

This equation was used to predict diffusion of erucamide in polyamide-12, PA-12, at three temperatures. Film containing 15 wt% erucamide was placed between erucamide-free films and diffusion was carried out under isothermal conditions. Figures 7.1 and 7.2 show some data. Experimental points (Figure 7.1) obtained from gas chromatographic determination of concentration of erucamide confirm that the concentration profile calculated from a simple Fickian diffusion (equation 7.1) is correct. 

Erucamide can also be conveniently determined by GC-MS or liquid chromatography mass spectrometry, LC-MS as was demonstrated for samples containing erucamide and thermal stabilizers. ... 

Microwave-assisted extraction was used to shorten sample preparation time for HPLC analysis. Results of determination were accurate in spite of the fact that sample grinding was omitted due to the novel method of extraction. In another study by HPLC, amides were extracted in a Soxhlet extractor from 3 cm wide strips, and excellent recovery was reported. Simultaneous determination of erucamide, oleamide, and stearamide was performed with good resolution, repeatability and reproducibility. ... 

XPS was used to determine erucamide concentration on the surface of LDPE film." The film samples were cut at the blown film production line and immediately frozen in dry ice." The samples were kept frozen until pseudo-real-time monitoring experiments were initiated." To ensure that the initial surface was fi ee of erucamide, the film was hurriedly rinsed with methanol." ... 

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