Document ID: chunk:federal_register_of_legislation:F2013C00288:reg:13:p2
Version: federal_register_of_legislation:F2013C00288
Segment Type: reg
Provision Reference: reg 13 (pt 2/9)
Character Range: 852929–856005

(LCS)  As a minimum, a laboratory control sample should be run with each batch of 20 samples. This quality control sample should be processed through the entire analytical method and reported with the data. The LCS is a clean soil fortified with the same hydrocarbon product mix as used for the CVS, or a reference sample with a consensus hydrocarbon value. Recovery of product should be checked by analysing either ethanol-free petrol or any other suitable product with predominant hydrocarbons in the nC6– nC10 range. The calculated LCS concentration should be between 70 and 130% of the expected concentration or a recovery range established by ongoing quality control charts.

    13.1.2     Method validation
The methods should be validated by each laboratory using them, in accord with this Schedule. Some method validation parameters require particular attention, as below.

13.1.2.1     Hydrocarbon product linearity
Establish linearity of the detector response using hydrocarbon products that cover the particular hydrocarbon fraction (for example, ethanol-free petrol for Method A1 (analysis of volatiles), or a mix of diesel and motor oil for Method A2, (analysis of semi-volatiles). Linearity should be within 15% in each of the calibrated carbon ranges. As a general principle, the peak height of the largest product component in a fraction should not exceed the peak height of the single n-alkane in the highest level calibration standard.

13.1.2.2     Product standard reference materials
A reference hydrocarbon product(s) should be prepared and analysed. The products(s) should cover the range of hydrocarbon fractions specified in this method. The product or products should be well characterised, such that the quantitative composition of the relevant fractions is known. This allows the assignment of a portion of a known quantity of this product to a particular fraction. This solution can then be ideally used as the CVS for ongoing quality control.

Accuracy of the method should be established by obtaining acceptable recoveries for hydrocarbons from a certified reference material (i.e. soil contaminated with hydrocarbons).

13.1.2.3     Proficiency studies
Ongoing participation in relevant proficiency studies is required to validate this method.

13.2          Method A1: Determination of volatile TRH: TRH C6 – C10

    13.2.1     Scope and application
This method is applicable to the determination of hydrocarbons eluting between nC6 and nC10 alkanes, inclusive of BTEX. Target compound analysis can occur simultaneously when running this method, provided that suitable specific detectors are employed, e.g. PID for aromatic compounds, or MS.

Note: Semi-volatile hydrocarbons with higher boiling points should be analysed by the TRH semi-volatile method (see Method A2 below (Section 14.3) and Section 11.13).

    13.2.2     Limitations
    * This method does not distinguish between petrogenic and biogenic compounds or synthetic compounds, such as chlorinated solvents; it measures the total recoverable hydrocarbons present, hence it is