Methods Manual

As part of the Technical Studies Program, NCASI sometimes develops methods for analytical parameters for which no rigorously tested or validated methods are available. Once developed, these NCASI methods are frequently used for other program applications and to respond to regulatory and member company requests. The methods are compiled into a single manual to facilitate their distribution and use.

Questions regarding the content of the NCASI Methods Manual may be directed to Terry Bousquet, Project Leader, at the NCASI West Coast Regional Center. Questions regarding specific method content should be directed to the originating NCASI center listed on the cover page of each method.

The manual is also available to Member Company Personnel on CD-ROM. Send your request to, or contact the NCASI Headquarters.


On this page:

I. Introduction

II. Water, Wastewater and Process Liquid Methods

Methods Manual (02.B.002): Method CP-86.07 Chlorinated Phenolics in Water by In-Situ Acetylation and GC/MS Determination

PDF      Published 03/2007 View Abstract

Method CP 86.07 is used to determine and confirm the concentrations of selected chlorinated phenols, chlorinated guaiacols, chlorinated catechols, chlorinated benzaldehydes (i.e., vanillins and syringaldehydes), and trichlorosyringol in extracts prepared from water samples by gas chromatography/mass spectrometry (GC/MS). This method is an updated version of NCASI Method CP 86.02 (NCASI 1986, 1997) which has been revised to meet the needs of the pulp and paper industry for the monitoring of chlorinated phenolics for the Cluster Rule ( Federal Register 1998). Modifications to the method include: (a) a reduced analyte list (nonchlorinated compounds removed); (b) the addition of acenaphthene–d10 as an internal standard for quantitation of 3,4,5 trichlorophenol (in situ derivatization internal standard), 3,4,5 trichlorocatechol 13C6 (surrogate), and 5 bromovanillin (surrogate); (c) the use of potassium carbonate to adjust sample pH; (d) the addition of 5 bromovanillin as a surrogate for the chlorovanillins; and (e) the addition of 3,4,5 trichlorocatechol 13C6 as a surrogate for the chlorocatechols. Section 17, Table 1 lists the compounds which can be confirmed or determined by this method.

Methods Manual (02.B.011): Method RSC-02.02 Reduced Sulfur Compounds by Direct Injection GC/PFPD

PDF      Published 03/2007 View Abstract

This method is used for the determination of the reduced sulfur compounds (RSCs) total sulfide as hydrogen sulfide (H2S) [7783-06-4], methyl mercaptan (MeSH) [74-93-1], dimethyl sulfide (DMS) [75-18-3], dimethyl disulfide (DMDS) [624-92-0], and dimethyl trisulfide (DMTS) [3658-80-8] in wastewaters from pulp and paper mills. The RSCs are measured by direct aqueous injection gas chromatography with pulsed flame photometric detection (GC/PFPD).

Methods Manual (02.B.012): Method HIMS-W106.01 Hexazinone, Imazapyr, Metsulfuron Methyl, and Sulfometuron Methyl in Water by Solid Phase Extraction and HPLC/UV

PDF      Published 02/2007 View Abstract

Method HIMS-W106.01 is applicable for the determination of dissolved concentrations of hexazinone (the active ingredient in Velpar®), imazapyr (the active ingredient in Arsenal®, Chopper®, and Assault®), metsulfuron methyl (the active ingredient in Escort® and Ally®), and sulfometuron methyl (the active ingredient in Oust® and Oustar®) in ambient waters. The general analytical approach used in this method is based on multiple literature reports (1,2,3).

Methods Manual (02.B.013): Method POLY-W109.01 Polyphenolics in Pulp Mill Wastewaters by Spectrophotometry

PDF      Published 11/2009 View Abstract

Method POLY-W109.01 procedures utilize a spectrophotometer to measure the absorbance of light as it passes through a sample that has been prepared by reaction with TanniVer 3® Folin phenol reagent. Concentrations of all hydroxylated compounds (polyphenols) that give a proportional blue color are determined by comparison of the absorbance of the sample to the absorbance of tannic acid solutions of known concentrations.

Methods Manual (02.B.014): Method TNTP-W10900 Total Nitrogen and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion

PDF      Published 06/2011 View Abstract

This method is applicable to determinations of total nitrogen (TN) and total phosphorus (TP) in acid preserved pulp, paper, and paperboard mill biologically treated effluent (PP BTWW). The applicable range of this method is 0.01 to 3.0 mg P/L and 0.1 to 6.0 mg N/L. The range may be extended with sample dilution. Sample size is 7 mL. Laboratories intending to use this procedure should establish method detection limits for each sample matrix type. Changes in technology may influence chemical compositions of these matrices, requiring evaluation of samples for digestion efficiency and method performance. Any modification of the method beyond those expressly permitted is subject to application and approval of alternative test procedures under 40 CFR Parts 136.4 and 136.5 (Section 16.1). The method simultaneously converts ammonia and inorganic (excluding N 2 ) and organic nitrogen to nitrate and inorganic and organic forms of phosphorus to orthophosphate by means of an alkaline to acid digestion. Native dissolved nitrate and nitrite are unaffected by the digestion.

III. Air Sampling Methods

IV. Workplace Sampling Methods

V. Appendices