Alcohol andGlycol

(Method 8015B)

Description

Method 8015B is used to determine Alcohol and Glycol in a variety of matrices. These methods are applicable to nearly all types of samples, including sludges, soils, sediments, extracts and waters. Examples of the common compounds would be methanol, ethanol, butanol, isobutanol, ethylene glycol and propylene glycol.

Semi-Volatile components are introduced into the GC by direct injection of either extraction solvent or the water sample itself. On a wide bore capillary column, the GC’s temperature is programmed to allow the column to separate the analytes. (See GC conditions Table III). Detection is achieved by flame ionization detector (FID).

Method sensitivity varies by matrix. The estimated quantitation limits on average are 2.0mg/Kg (wet weight) for soils, 2-100mg/Kg (wet weight) for wastes and 1.0mg/L for waters and extracts.

Apparatus and Materials

-Injector: Packed Column Injector

-Column: RTX-1, #30M, 0.53mmIDwith 1.5m film thickness for Alcohols,

Nukol 15M, 0.53mmID and 0.5m film thickness for Glycols

-Gas Chromatograph: HP 5890 Series II

-Data System: HP Chemstation

-FID detector

Reagents and Standards

-Standards are purchased as certified solutions or made by using an analytical

balance to weigh neat material

-Surrogates: Not applicable to this method

-Calibration Standards: Calibration standards at a minimum five

concentration levels are prepared. One standard must be at or near, but above the method detection limit. Calibration standards are prepared daily as required.

-Prepare calibration standards from purchased stock of 10,000g/mL by serial

dilutions.

-Matrix Spike Standard: Prepare prepared stock 10,000g/mL by diluting from a

second source.

-Laboratory Control Sample (LCS). Matrix spiking standard is used for LCS

-CCC Standard – Mid-level standard from a second source.

Note: All standards are stored at –10°C to –20°C in amber bottles with Teflon-

lined screw caps. All stock standards are stable for six months.

Procedure

1.0Initial Calibration

1.1Perform required preventative maintenance including injector liner, septa and replacement and column reconditioning, FID cleaning.

1.2Run calibration standards at a minimum of five concentrations. See Table IV.

1.3Calculate response factors (RF) for each compound in the standard set. See Table I.

1.4Based on the five calibration standards and the RF’s calculated in step 1.3, determine the average RF for each compound.

1.5Based on the RF values calculated in step 1.3, determine the %RSD for each compound. See Table V. The %RSD should be <20% for each compound.

2.0Daily Calibration

2.1Perform required preventative maintenance including injector liner, septa and replacement and column reconditioning, FID cleaning.

2.2Prepare and inject a mid-level standard and surrogates to verify initial calibration curve.

2.2.1Based on the continuing calibration standard, check the percent difference of RF for compounds, it must be +/- 15% of the initial calibration curve.

2.3Retention times must be monitored for the continuing calibration standard.

3.0Sample Analysis

3.1Extraction via liquid/liquid or sonication which is directly injected onto the capillary column, via the auto sampler.

4.0Data Analysis

4.1Each sample inject is reviewed and quantitated.

4.2If the response to any compound is greater than the initial calibration curve, dilutions must be made and re-analysis must be done.

4.2.1When evaluating data associated with saturated peaks a critical evaluation of carry over must be made. If carry over is suspected, re-analysis is required.

5.0Batch Acceptance Criteria

5.1All parameter detailed in the initial calibration (section 1.0) and daily calibration (section 2.0) must be met.

5.2In addition to the instrument performance outlined in the pervious step, the batch QC parameters for spike/spike duplicate and sample duplicates must be evaluated. The current acceptable limits are presented in Table I, VII and attachment 0140.

6.0Reporting of Results

6.1All results for QC parameters and samples are reported on the batch Queue list.

6.1.1All results are reported to three significant figures.

6.2Record instrument performance QC data on the daily validation report sheet. File all raw data along with complete form by date of analysis.

Quality Control

  • Initial Calibration parameters must be met after major maintenance, failed QC

or yearly

  • A daily check is required of all target compounds. Failure to meet quality control acceptable limits requires corrective action.
  • Each analytical batch analyzed must be accompanied by a blank consisting of ultra-pure water taken through all analytical steps.
  • All weights, volumes, comments, etc. for each batch must be entered in notebook form for data review.
  • As determined by notebook order, every 10th sample of similar matrix shall be analyzed in duplicate, every 20th sample shall be analyzed as a duplicate spike. (Calculations for RPD and % Recoveries must be calculated for each parameter, see procedure 0110 for calculations)
  • A laboratory control sample (LCS) must be analyzed per each analytical batch. The LCS consists of an aliquot sample of a clean control matrix similar to the sample matrix. The LCS is spiked with the same analytes at the same concentration as the matrix spike. When the results of the matrix spike analysis indicates a problem, the LCS results are used to verify that the laboratory can perform the analysis in a clean matrix.
  • Failure to meet quality control acceptable limits requires corrective action (see procedure 0150). Require, locate, and correct the source of the problem and repeat the test. Failure to meet the quality control acceptable limits again will require new calibration curve

References:

SW 846 Method 8021B pp8021B-1 to 8021B-19

Revision 2 December 1996

40 CFR PT 136 App. A Method 602 pp. 304-309









Procedure 0500

Revised 02/04