ANALYTICAL CASE STUDIES

Unique Environmental Testing

Summary:

Effluent waste water from an industrial facility showed elevated levels of a regulated priority pollutant; N-nitrosodiphenylamine. This analyte is typically examined as part of the standardized testing for semivolatile organic compounds (SVOC) using Gas Chromatography-Mass Spectrometry (GC-MS). This is described in EPA method 8270. However N-nitrosodiphenylamine can not be distinguished from the structurally similar diphenylamine. IsleChem was able to develop analysis technique using Liquid Chromatography-Mass Spectrometry (LC-MS) that allows for speciation of these two compounds.

GC-MS shows only a single species for a mix of N-nitrosodiphenylamine and diphenylamine. The nitroso compound thermally rearranges in the GC injection port to form diphenyl amine.

LC-MS allows for speciation and can achieve comparable reporting limits.

Benefits:

  • Quantitative results were accepted by regulatory authorities
  • Facility demonstrated that priority pollutant concentration in their effluent was below regulatory limits
  • Experience of staff able to use unique Analytical tools to solve environmental issues

 

 

Evaluation of Chemical Raw Materials

Summary:

A manufacture of pool chemicals used as disinfecting agents wanted to change suppliers of a critical raw material. Manufacture wanted to ensure that chemical composition and physical properties were equivalent to current supplier. IsleChem performed the following testing comparing current and new supplier.

Parameter Analytical Technique
Assay HPLC
Organic Impurities HPLC
Trace Metals ICP-OES
Bulk Density Gravimetric
Moisture Karl Fisher Titration
Granulation / Particle Size Sieves
Physical Appearance Color Comparison

Benefits:

  • Data set showed raw material was comparable to current supplier
  • Client established raw material Quality Control (QC) specification
  • Switch to new supplier resulted in significant cost savings and provided a dual source raw material supplier

 

 

Volatile Organic Compounds (VOC) Testing in Surface Coatings

Summary:

Commercial paints and coating are regulated by the US EPA for VOC content.1Client suspected that based upon cost comparison a competitor’s product was not did not meet VOC regulations. Formulations for these materials can be complex and contain both exempt and non-exempt solvents. Compliance testing is required and must be performed in accordance with guidelines in US EPA Method 24. This method utilizes ASTM specified procedures which include:

Heading Heading
Density ASTM D 1475
Water Content ASTM D 4017
Total Volatile Content ASTM D 2369
Volatile Organic Compounds ASTM D 6886-03

IsleChem employed Gas Chromatography-Mass Spectrometry (GC-MS) as the tool of choice to identify VOCs. This allowed for the disposition of solvents; exempt or non-exempt. This is followed by quantification using GC to determine total content of all non-exempt VOCs.

GC-MS of a commercial coating used to seal concrete.
Peaks identified as:
-1.66 min. Acetone (an exempt solvent)
- 7.21, 7.51 and 7.91-min. – Xylenes (non-exempt solvent)

Benefits:

  • Customer was able to submit data to EPA that questions their competitors claim that they were COC compliant.
  • GC-MS testing can provide insight into what VOCs are used in the marketplace in coatings and paints.
  • Valued information can be applied to formulating / re-formulating products

ENVIRONMENTAL PROTECTION AGENCY, 40 CFR Part 59 [AD–FRL–6149–7], RIN 2060–AE55 "National Volatile Organic Compound Emission Standards for Architectural Coatings", Environmental Protection Agency (EPA), Final rule. Subsection 59.406 (a) (1) - Compliance provisions

 

 

Identification of a Surface Contaminant on Food Packaging Material

Summary:

Packaging used for food is constructed of a multi-layer composite intended to preserve contents, form a barrier to the environment and act as a sub straight for printing. IsleChem was commissioned to investigate poor print quality on such packaging material. After a discussion with the Client it was discovered poor print quality was linked to material that went through a specific roll mill to form the laminate. A surface contaminant was suspected. After solvent extraction of the packaging material the extract was examined by Fourier Transform-Infrared (FT-IR) Spectrophotometry. Resulting spectrum was compared with reference spectra and was identified as a fatty acid amide; erucamide

FT-IR of solvent extract from food packaging (top) and reference spectrum of a fatty acid amide (bottom).

Benefits:

  • IsleChem was able to ID a surface containment commonly used as a anti-adhesion / slip agent
  • Client found that this compound was in use in the production of food packaging, specifically to the roll mill that yield poor print quality material.
  • Study lead to implementation of alternative slip agents there by eliminating print quality related issues

 

 

Polymer Characterization for Molecular Weight Distribution Values

Production of a low molecular weight polyisobutylenes used in an adhesive application showed poor performance. IsleChem performed Gel Permeation Chromatography (GPC) to obtain molecular with distribution values of Mp, Mn, Mw and Mz. Comparison was made with a control product showing consistent good adhesive properties.

Overlay GPC of two low molecular weight polymers showing varied adhesive properties

Sample Mp Mn Mw Mz
Control polymer 1 3700 2800 5000 8800
polymer 2 2100 1200 4000 7000

Benefits:

  • IsleChem demonstrated good correlation with observed adhesion and the materials molecular weight.
  • Client incorporated GPC technique at their facility as a Quality Control monitoring tool

 

 

Assay of Pharmaceutical Antibiotics

Summary:

A supplier of pharmaceutical antibiotics requested third party testing following U.S. Pharmacopoeia (USP) methodologies. Upon HPLC/UV assay analysis of a particular lot of one of the antibiotics undergoing testing, a slight variation in retention time was observed for that lot material relative to that of the certified reference standard for that antibiotic. The sample was re-analyzed using HPLC/DAD and it was positively determined that the particular lot sample was in fact not the antibiotic expected.

Spectrum of suspect antibiotic lot sample.

Chromatogram of suspect antibiotic lot sample.

Spectrum of USP Reference Standard of expected antibiotic.

Chromatogram of USP Reference Standard of expected antibiotic.

Benefits:

  • Client did not distribute wrong antibiotic to their customers.
  • Client was able to contact their manufacturer to inform them of error and re-coup costs of material.
  • The chromatographer suspected something amiss with sample, and quickly confirmed that the antibiotic sample was not what it was labeled as. Third party verification by experienced analytical laboratory staff saved a potentially catastrophic accident from occurring, had the miss-indentified antibiotic been distributed.

 

 

Plating Bath Balance Issue

Summary:

A printer using nickel plating baths to make master plates was experiencing a number of quality issues with the finished plates. A field consultation was held at the printing facility to discuss the problem and view finished plates, and to examine and discuss the chemistry and operational parameters of the plating baths. Samples of the baths were taken and evaluated, and it was determined that the chemistry of the nickel baths was out of balance, with nickel being low and boric acid relatively high. This in turn caused the finished plates to have flaws and/or prematurely fail.

The customer was trained on-site how to easily and quickly monitor the chemistry of their tanks. A spreadsheet was also created for the customer to automatically calculate which and how much replenishment reagents to add to regain proper levels and balance, based upon tank volume, operating temperature, nickel, boric acid and pH values obtained from the on-site monitoring.

Specific metal titration with colored endpoint (example – used to measure exact nickel or boric acid concentration in plating baths).

Hydrometer testing to quickly measure specific gravity of plating baths (indicator of total dissolved solids).

Benefits:

  • Client corrected problems with master plates.
  • Client trained to collect real-time profile of plating baths, with on-site chemistries being evaluated at a frequency required to assure correct operation of the plating baths.
  • Client periodically sends in bath samples for analyses to assure that on-site analyses are being performed correctly and any reagents used in the analyses are still acceptable.
  • Spreadsheet developed allows bath operator to quickly re-adjust plating bath chemistry for volume, temperature or chemical balance.

 

 

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