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Laboratory Services


A Review of Analytical Methodologies in PM Analysis
This paper was presented by Dr. Malkit Basi, Laboratory Manager and Technical Director
of Ledoux & Company, at the June 2006 IPMI Conference.

Ledoux & Company is ISO 9001-2000 certified

 

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Laboratory services generally fall into 2 main groups—that is party or control assays and umpire or referee assays. Ledoux’s reputation as an umpire laboratory is well known to the industries that we have serviced for so many years. For umpire assays, our methods are more rigorous, generally involving different methods with different chemists responsible and certainly more portions. As splitting limits have gotten so narrow over the years, umpiring between them is becoming increasingly more difficult because of analytical differences. You can very easily see that only certain laboratories with the proper resources will be able to provide what is expected. As you would expect, the majority of our referee assays are in the precious metal elements.

Ledoux and Company routinely use Fire Assay, Clasical Wet Chemistry and Instrumental Analysis as appropriate to provide a representative assays for major and minor constituents in your material.
Methods employed for assay purposes are dependant on the type of material and the size of a particular lot. Please contact Dr. M.S. Basi: (mbasi@ledoux.com) if you need to discuss any aspects of assays recommended for your material prior to submitting samples. The merits and applicability of some of the techniques used everyday at Ledoux and Co are summarized in the following sections.


Fire Assay

Ledoux and Company provides comprehensive fire assay facilities for the determination of precious metals in a variety of materials. The method is capable of extracting milligram or even microgram amounts of gold, silver and other precious metals from even the most complex matrices. The technique is rigorously tested and proven to be accurate and reliable. It is accepted as the method of choice for commercial assays. Applications include :
• Gold and silver assays for commercial trade.
• Precious metal determination in scrap and sweeps from the jewelry industry.
• Evaluation of ores and concentrates.
The laboratory is well equipped with two fusion furnaces, and two cupellation furnaces for lead fire assay work as well as 2 cupellation furnaces for gold and silver assay
Two additional fusion furnaces are available for Nickel sulfide and Copper sulfide collections.
Fire Assay personnel at Ledoux and Co are well trained professionals with many years of experience.
The Company has offered this type of expertise to the industry throughout the last century.


Wet Chemistry


Our wet chemistry section is made up of a base metal department, a reforming catalyst section, an automotive catalyst department and a Precious Metal department.

For precious metals in the trace to few percent range, our analysts will perform separations, then the solutions go to our ICP department for measurement.
The company has 3 ICP Emission Spec units and one ICP Mass Spec unit.
For the higher grades, after separation, generally gravimetric methods are preferred for the precious metals, and titrimetric methods for the base metals.

Instrumental Analysis

Instrumental techniques are used where appropriate for quantification. In this way results can be provided to the client at an affordable price in a less time that will normally be required by classical assays. Even in this case initial sample preparation and separation of the elements of interest is very often necessary to achieve the quality that the industry has become accustomed from a major independent Lab like Ledoux and Company.
  • Reforming Catalysts
  • Autocatalysts
  • Mineral and Geological Materials.

Trace element and trace impurity analysis

Trace element and trace impurity analysis includes all naturally occurring elements in diverse matrices. Major constituents in a variety of materials can also be determined. Various instrumental techniques are employed. However X-ray Fluorescence, plasma emission spectrometry and atomic absorption have become especially popular over the years. Some of these techniques and their capabilities have been described below:

Applications:

  • Solutions:
    Direct solution analysis is carried out in some cases. Very often some type of pretreatment is necessary. It may include sample dilution, matrix matching, internal reference addition etc.
  • Metals:
    Dissolution in appropriate acid is the minimum requirement. Trace constituents may need a chemical separation and pre-concentration for accurate determination.
  • Powders:
    Catalysts, precious metal containing materials, minerals and geological materials require complex sample handling before presentation for plasma emission analysis. Wet chemical or fire assay separations are very often needed to produce an accurate analysis.


Type of materials submitted for assay include:

  • Bullion, metal and dore.
  • Scrap and sweeps from the jewelry industry.
  • Ores and concentrates.
  • Catalysts.

We also have the capability to test for halides with our Ion Chromatography equipment. We can also test for carbon and/or sulfur with our Carbon Sulfur Analyzer. Ledoux & Company also has an X-ray Fluorescence Unit capable of fast, non-destructive qualitative to semi-quantitative analysis. This helps to assign samples by identifying the matrix and relative concentration of the elements present. Accurate quantitative analysis can be accomplished if proper reference standards are available.

Ledoux & Company is an ISO 9001-2000 registered company since 2003.
Having now been through three semi-annual audits, we are keenly aware of what is expected as it pertains to documentation and quality programs from a laboratory providing services on an international basis.
Whether or not being ISO certified is important to you specifically, we cannot know, except to state that such certification implies that we have methods and operational procedures that are written, and followed, and that when change is necessary or errors/complaints occur, as they always do, that such is documented and remedied if necessary.

Through Ledoux's industry alliances, we have additional sampling capabilities on a national level via locations from New York to California. At the international level, Ledoux has representation in Belgium, Canada, France, Germany, Japan, Russia, Spain, Sweden, and the United Kingdom.

 
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