**SW-846 Update V 8430 - 1 Revision 1 July 2014**  **METHOD 8430**

**ANALYSIS OF BIS(2-CHLOROETHYL) ETHER AND HYDROLYSI S PRODUCTS** 
**BY DIRECT AQUEOUS INJECTION GAS CHROMATOGRAPHY/FOUR IER TRANSFORM** 

**INFRARED**

**1.0 SCOPE AND APPLICATION**

**1.1 This method provides procedures for the identif ication and quantitation of bis(2-**  **chloroethyl)ether and its hydrolysis compounds in a queous matrices by direct aqueous injection**  **(DAI) into a gas chromatograph with detection by a Fourier transform infrared spectrometer**  **(GC/FT-IR). The following compounds can be determi ned by this method:** 

**Compound Name Abbreviation CAS Number a** 

**Bis(2-chloroethyl)ether BCEE 111-44-4**

**2-Chloroethanol CE 107-07-3**
**2-(2-Chloroethoxy)ethanol 2CEE 628-89-7**
**Diethylene glycol DEG 111-46-6**
**Ethylene glycol EG 107-21-1**

**a Chemical Abstract Service Registry Number.** 

**1.2 Although the initial study upon which this met hod is based targeted only the bis(2-**  **chloroethyl)ether and its hydrolysis compounds, it has been suggested that this method can be**  **used for the identification of compounds that are g enerally non-extractable, highly water soluble,**  **thermally stable, and do not co-elute with water fr om the gas chromatography (GC). Possible**  **analytes include ethers and alcohols.**

**1.3 The minimum identifiable quantities (MIQ) for the five compounds in organic-free**  **reagent water range from a low of 46 ng for BCEE, t o a high of 120 ng for EG (See Sec. 13.2 for**  **MIQ definition). The MIQ for a specific sample may differ depending on the nature of the**  **interferences in the sample matrix and the amount o f sample used for the analysis.** 

**1.4 This method is restricted to use by or under t he supervision of analysts**  **experienced in the use of a GC, the interpretation of FT-IR spectra and the use of continuous**  **data collection systems. Each analyst must demonst rate the ability to generate acceptable** 

**results with this method.**

**2.0 SUMMARY OF METHOD**

**2.1 Water samples are filtered through a 0.45-μm f ilter, and 1-μL aliquots are injected**  **directly into a GC. The GC is equipped with two de tectors, a thermal conductivity detector**  **(TCD) and an FT-IR. During analysis, the analyst d isconnects the FT-IR from the system to**  **prevent aqueous degradation of the potassium bromid e (KBr) window, using an eight-port**  **switching valve. Further analysis of either the so lid precipitate from the filtering step or the**  **aqueous filtrate for trace amounts of non-water sol uble compounds may be done by extracting**  **the samples using appropriate 3500 series methods. SW-846 Update V 8430 - 2 Revision 1**  **July 2014 3.0 DEFINITIONS** 

**Refer to Chapter One, the individual determinative methods, and the manufacturer's**  **instructions for definitions that may be relevant.**

**4.0 INTERFERENCES**

**4.1 Method interference may be caused by contamina nts in solvents, reagents,**  **glassware and other sample processing hardware that lead to discrete artifacts and/or elevated**  **baselines in the chromatograms. All of these mater ials must be routinely demonstrated to be** 

**free from interferences under the conditions of the analysis by running laboratory method** 

**blanks.**

**4.1.1 Glassware must be scrupulously cleaned. Cl ean all glassware as soon**  **as possible after use by rinsing with the last solv ent used. This should be followed by**  **detergent washing with hot water, and rinses with t ap water and organic-free reagent**  **water. It should then be drained dry, and heated i n a laboratory oven at 130 °C for several**  **hours before use. Solvent rinsing with methanol ma y be substituted for the oven heating.**  **After drying and cooling, glassware should be store d in a clean environment to prevent**  **any accumulation of dust or other contaminants.**

**4.1.2 The use of high purity reagents and solvent s helps to minimize**  **interference problems. Purification of solvents by distillation in all-glass systems may be**  **required.**

**4.2 Matrix interferences may be caused by contamin ants that are in the sample. The**  **extent of matrix interferences will vary considerab ly from source to source, depending upon the**  **nature and diversity of the matrix being sampled. If significant interferences occur in**  **subsequent samples, additional cleanup may be neces sary.** 

**4.3 The extent of interferences that may be encoun tered in this method has not been**  **fully assessed. Although the GC conditions describ ed allow for a unique resolution of the**  **specific compounds covered by this method, other ma trix components may interfere.** 

**5.0 SAFETY**

**This method does not address all safety issues asso ciated with its use. The laboratory is**  **responsible for maintaining a safe work environment and a current awareness file of**  **Occupational Safety and Health Administration (OSHA ) regulations regarding the safe handling** 

**of the chemicals and instrumentation included in th is method. A reference file of material safety**  **data sheets (MSDSs) should be available to all pers onnel involved in these analyses.** 

**6.0 EQUIPMENT AND SUPPLIES**

**6.1 GC/FT-IR system**

**6.1.1 GC – Temperature-programmable oven equipped with a cool on-column**  **injection port, a purged splitless injection port, or an equivalent suitable for capillary glass** 

**columns SW-846 Update V 8430 - 3 Revision 1**  **July 2014 6.1.2 Column – 30 m DB-wax, 1.0 μm film, Megabore**  **(J&W Scientific), or equivalent** 

**6.1.3 Detectors**

**6.1.3.1 TCD – Must be able to handle temperature s up to 300 °C** 

**6.1.3.2 FT-IR spectrometer – System should be eq uipped with a** 

**mercury-cadmium-telluride detector, using a light-p ipe interface with KBr windows**  **(i.e., Digilab Model GC/C32 or equivalent). Resolu tion of 8 cm**  **-1 and a range of**  **4,000 to 7,000 cm -1**  **is required. The light-pipe interface and transfe r lines should**  **be contained in a heated system (up to 250 °C) to p revent sample condensation.** 

**Extra transfer lines will be needed for the switchi ng system.** 

**6.1.4 Detector switching system – Eight-port stai nless steel GC rotary switching**  **valve, with an inert interval surface (e.g., front end processor (FEP)) and capable of**  **withstanding temperatures up to 300 °C. Ideally, t he valve should be mounted inside the** 

**GC oven with external control. If internal mountin g is not possible, then use of an external**  **heated valve enclosure may be employed. This allow s direct injection of aqueous**  **samples by using the valve system to route water aw ay from the FT-IR KBr window, which**  **water rapidly destroys.**

**6.1.5 Data collection – Each detector should have its own signal recorder.** 

**6.1.5.1 TCD signal – Either an analog strip char t recorder or a digital**  **computerized data collection system is acceptable.**

**6.1.5.2 FT-IR signal – The continuous collection of the spectrometer's** 

**signal will require a computerized data system with the ability to continuously**  **collect spectra at a rate of 4 scans/sec and add th e 4 scans to produce a data point**  **for each second. To confirm the identity of target compounds, a library of vapor**  **phase spectra should be established.**

**6.2 Glassware**

**6.2.1 Glass funnels**

**6.2.2 Volumetric flasks (square) – various sizes**

**6.2.3 Pipettes (A grade) – various sizes**

**6.2.4 Sample vial with polytetrafluoroethylene (P TFE)-lined lids** 

**6.3 Syringes – 10 μL, suitable for GC work**

**6.4 Analytical balance, accurate to ±0.0001 g**

**6.5 Vacuum filtration apparatus – 0.45 μm filter a nd clean glass flasks that are able to**  **hold at least 1 L of liquid SW-846 Update V 8430 - 4 Revision 1**  **July 2014 7.0 REAGENTS AND STANDARDS** 

**7.1 Reagent-grade chemicals shall be used in all t ests. Unless otherwise indicated, it**  **is intended that all reagents shall conform to the specifications of the Committee on Analytical**  **Reagents of the American Chemical Society (ACS), wh ere such specifications are available.**  **Other grades may be used, provided it is first asce rtained that the reagent is of sufficiently high**  **purity to permit its use without lessening the accu racy of the determination.** 

**7.2 Organic-free reagent water – All references to water in this method refer to**  **organic-free reagent water, as defined in Chapter O ne.** 

**7.3 Helium gas – Suitable for gas chromatography**

**7.4 Methanol, CH 3**  **OH – Pesticide reagent grade, nanograde, or equival ent** 

**7.5 Stock standard solutions**

**7.5.1 Prepare, in organic-free reagent water, a s tock standard solution**  **containing all of the target analytes at a concentr ation of 1000 mg/L. Record the actual**  **weight of each compound added and calculate the act ual concentration of each**  **component of the solution.**

**7.5.2 Transfer the stock standard solution into a PTFE-sealed screw-cap bottle**  **for storage. Store at ≤6 °C and protect from light . Check the solution periodically for signs**  **of degradation or evaporation. This solution must be replaced every three months, or**  **when any sign of degradation or evaporation is obse rved.** 

**7.6 Calibration standards**

**7.6.1 Calibration standards at 500, 250, 100, 50, and 25 mg/L, from the**  **aqueous stock standard solution, by appropriate vol umetric dilutions with water are**  **suggested. Store as specified in Sec. 7.5.2. The calibration solutions should not be made**  **by serial dilution of a single solution.**

**7.6.2 Since the levels of detection for the targe t compounds in water have not**  **been established, the suggested calibration curve c oncentrations may be modified,**  **depending on matrix interferences and sensitivity o f equipment. In general, the calibration**  **curve should span at least one order of magnitude a nd the working range should bracket**  **the analyte concentration.**

**7.7 Spiking solution – The analyst should monitor the performance of the analytical**  **system and the effectiveness of the method in deali ng with each sample matrix, by spiking a**  **known amount of the target analytes into blanks or into matrix spike samples. A suggested**  **preliminary concentration of the spiking stock solu tion is 100 g/L. It is recommended that the**  **spiking concentration should be set at 1 to 5 times higher than the background concentration** 

**determined for that matrix.**

**7.8 Surrogate spiking solution – To monitor the pe rformance of the method for all**  **samples, a minimum of one surrogate compound should be chosen by the laboratory. This**  **compound should be diluted with water to an appropr iate concentration and added to all**  **samples, method blanks, matrix spikes, and calibrat ion standards.** **SW-846 Update V 8430 - 5 Revision 1 July 2014**  **8.0 SAMPLE COLLECTION, PRESERVATION AND HANDLING**

**8.1 See Chapter 4, Organic Analytes, Sec. 4.1 for more information on this topic.** 

**8.2 Samples should be stored at ≤6 °C and protecte d from light.** 

**8.3 Samples should be filtered and analyzed within 14 days of collection.** 

**9.0 QUALITY CONTROL**

**9.1 General guidance**

**Refer to Chapter One for guidance on quality assura nce (QA) and quality control (QC)**  **protocols. When inconsistencies exist between QC g uidelines, method-specific QC criteria take**  **precedence over both technique-specific and Chapter One criteria; technique-specific QC**  **criteria take precedence over Chapter One criteria. Any effort involving collection of analytical**  **data should include development of a structured and systematic planning document, such as a**  **quality assurance project plan (QAPP) or a sampling and analysis plan (SAP), which translates**  **project objectives and specifications into directio ns for those who will implement the project and** 

**assess the results.**

**Each laboratory should maintain a formal QA program . The laboratory should also maintain**  **records to document the quality of the data generat ed. Development of in-house QC limits for**  **each method is encouraged, as described in Sec. 9.6 of Method 8000. Use of instrument**  **specific QC limits is encouraged, provided such lim its will generate data appropriate for use in**  **the intended application. All data sheets and QC d ata should be maintained for reference or**  **inspection. QC to validate sample extraction is co vered in Method 3500 and in the extraction**  **method utilized. If extract cleanup was performed, follow the QC in Method 3600 and in the**  **specific cleanup method.**

**9.2 Initial demonstration of proficiency (IDP)**

**Prior to implementation of a method, each laborator y must perform an IDP consisting of at**  **least four replicate reference samples spiked into a clean matrix taken through the entire**  **sample preparation and analysis. Whenever a signif icant change to instrumentation or**  **procedure occurs, the laboratory must demonstrate t hat acceptable precision and bias can still**  **be obtained by the changed conditions. Whenever ne w staff members are trained, an analyst**  **IDP must be performed.**

**9.2.1 Demonstration of proficiency for new analysts**

**Each laboratory should have a training program whic h documents that a new**  **analyst is capable of performing the method, or por tion of the method, for which the**  **analyst is responsible. This demonstration should document that the new analyst is**  **capable of successfully following the standard oper ating procedure (SOP) established by**  **the laboratory.**

**9.3 It is recommended that the laboratory adopt add itional QA practices for use with**  **this method. The specific practices that are most productive depend upon the needs of the**  **laboratory and the nature of the samples. Whenever possible, the laboratory should analyze**  **standard reference materials and participate in rel evant performance evaluation studies.** **SW-846 Update V 8430 - 6 Revision 1 July 2014**  **9.4 Lower limit of quantitation (LLOQ)**

**The laboratory shall establish the LLOQ as the low est point of quantitation, which**  **in most cases, is the lowest concentration in the c alibration curve. LLOQ verification is**  **recommended for each project application to validat e quantitation capability at low analyte**  **concentration levels. This verification may be acc omplished with either clean control material**  **(e.g., reagent water, solvent blank, Ottawa sand, d iatomaceous earth, etc.) or a representative**  **sample matrix, free of target compounds. Optimally , the LLOQ should be less than the desired**  **regulatory action levels based on the stated data q uality objectives (DQOs).** 

**9.5 QC necessary to evaluate the GC system operati on is found in Method 8000 Sec.**  **11 under Retention Time Windows, Calibration Verifi cation and Chromatographic Analysis of**  **Samples. Refer to Table 1 for FT-IR spectrometer Q C requirements.** 

**9.6 Sample QC for preparation and analysis – The l aboratory should also have**  **established procedures for documenting the effect o f the matrix on method performance (i.e.,**  **precision, accuracy, and sensitivity). At a minimu m, this includes a method blank, matrix spike,**  **duplicate, and laboratory control sample (LCS) in e ach analytical batch and the addition of**  **surrogates to each field sample and QC sample(s).**

**9.6.1 Documenting the effect of the matrix should include the analysis of at**  **least one matrix spike and one duplicate unspiked s ample or one matrix spike/matrix spike**  **duplicate pair. The decision on whether to prepare and analyze duplicate samples or a**  **matrix spike/matrix spike duplicate should be based on knowledge of the samples in the**  **sample batch. If samples are expected to contain t arget analytes, then laboratories may**  **use one matrix spike and a duplicate analysis of an unspiked field sample. If samples are**  **not expected to contain target analytes, the labora tories should use a matrix spike and**  **matrix spike duplicate pair.**

**9.6.2 A LCS should be included with each analytic al batch. The LCS consists**  **of an aliquot of a clean (control) matrix similar t o the sample matrix and of the same weight**  **or volume. The LCS is spiked with the same analyte s at the same concentrations as the**  **matrix spike. When the results of the matrix spike analysis indicate a potential problem**  **due to the sample matrix itself, the LCS results ar e used to verify that the laboratory can**  **perform the analysis in a clean matrix.**

**9.6.3 See Method 8000, Sec. 9 for the details on carrying out sample QC for**  **preparation and analysis.**

**9.7 Surrogate recoveries – The laboratory should e valuate surrogate recovery data**  **from individual samples versus the surrogate contro l limits developed by the laboratory.**  **Currently, surrogate compounds have not been select ed for this procedure. See Method 8000,**  **Sec. 9 for information on evaluating surrogate data and developing and updating surrogate** 

**limits.**

**9.8 It is recommended that the laboratory adopt ad ditional QA practices for use with**  **this method. The specific practices that are most productive depend upon the needs of the**  **laboratory and the nature of the samples. Whenever possible, the laboratory should analyze**  **standard reference materials and participate in rel evant performance evaluation studies.** **SW-846 Update V 8430 - 7 Revision 1 July 2014**  **10.0 CALIBRATION AND STANDARDIZATION**

**10.1 External calibration – Calibration standards may be prepared using the suggested** 

**concentrations in Sec. 7.6. Matrix interferences m ay prevent quantitation at the suggested**  **concentrations. When necessary, the lowest concent ration of the calibration curve should**  **be adjusted to be at, or near, the LLOQ. Refer to Method 8000, Sec. 11 for proper**  **external calibration procedures.**

**10.2 Calibration must take place using the same sam ple introduction method that will be**  **used to analyze actual samples.**

**11.0 PROCEDURE**

**11.1 GC/FT-IR conditions (recommended):**

**Flow Rate: 2.4 mL/min of helium carrier gas Run Time: approximately 15 min**  **Injection Volume: 1 μL**

**Valve Switch Time: 4 min Temperature Program: 80 °C to 220 °C at 15 °C/**  **min, hold at 220 °C**

**for 10 min TCD Temperature: 290 °C**  **GC/FT-IR Interface, Transfer Lines, and**  **Light Pipe Temperature: 220 °C**

**Scan Time: 4 scans/sec**

**NOTE : Modifications of these parameters may be necessar**  **y to facilitate the separation of certain compounds depending on matrix interfere**  **nces encountered.**

**11.2 Refer to Method 8000, Sec. 11 for the establi shment of retention time windows.** 

**11.2.1 Analyze a solvent blank to ensure that the system is clean and** 

**interference free.**

**11.2.2 Analyze the 5 calibration standards, start ing with the lowest concentration**  **and ending with the highest concentration.**

**11.2.3 Tabulate the IR absorbance peak area along with the calibration factor**  **(CF) for the analyte at each concentration. Refer to Sec. 11 of Method 8000 for linear and**  **non-linear calibration acceptance criteria. It sho uld be noted that IR transmission is not**  **directly proportional to concentration.**

**11.2.4 Recheck the instrument calibration each da y, before and after an analysis**  **is performed, by analyzing one or more calibration standards. The response obtained**  **should fall within ±15 percent of the expected valu e or the instrument must be recalibrated.** 

**11.2.5 After the analysis of 10 or fewer samples, one of the calibration standards**  **must be reanalyzed to ensure that the retention tim es and the CFs of the target analytes**  **remain within the QC requirements.**

**11.3 Sample spiking and filtering SW-846 Update V 8430 - 8 Revision 1**  **July 2014 11.3.1 Allow the sample to come to ambient temper**  **ature. Mark the water meniscus on the side of the 1-L sample bottle for l**  **ater determination of exact sample**

**volume.**

**11.3.2 Add 2 mL of the spiking solution to the sp iked blank and the matrix spike**  **sample. The final concentration of the added analy tes should be approximately 200 mg/L.** 

**11.3.3 Vacuum filter the sample through a 0.45-μm filter that has been rinsed**  **with organic-free reagent water. The filtrate shou ld be collected in a clean glass bottle.**  **Any particulate collected by the filtering process may be discarded or extracted for**  **analysis of trace amounts of non-water soluble comp ounds using an appropriate 3500** 

**series method.**

**11.3.4 Using a pipette, withdraw a 5-mL aliquot o f the sample (aqueous filtrate)**  **and place it into a clean glass sample vial with a PTFE-lined lid. This 5-mL aliquot will be**  **the sample used for the direct aqueous injection of the water sample. Store sample** 

**extracts at ≤6 °C in the dark. The remainder of th e aqueous filtrate may be saved in a**  **glass bottle with a PTFE-lined lid until after the analysis is complete or extracted for**  **analysis of trace amounts of non-water soluble comp ounds using an appropriate 3500** 

**series method.**

**11.4 GC analysis**

**11.4.1 Method 8000, Sec. 11 provides instructions on calibration, establishing**  **retention time windows, the analysis sequence, appr opriate dilutions, and**  **chromatographic identification criteria.**

**11.4.2 Determining the valve switching time – The valve switch time must be**  **determined before proceeding with the analysis of s amples.** 

**11.4.2.1 Place the GC switching valve in the pos ition which routes the** 

**sample to the TCD and away from the FT-IR spectrome ter and inject a 1 μL aliquot**  **of a reagent blank to determine the retention time of water in the system. Use this**  **retention time to determine the optimum valve switc h time to cycle water away from**  **the KBr window loop. At the optimum valve switch t ime, the eight-port valve may**  **be moved to the position which allows use of the FT -IR detector and the TCD in**  **tandem after the bulk of the aqueous portion of the sample has been diverted away** 

**from the KBr window.**

**11.4.2.2 Once the optimum valve switch time is e stablished, the system** 

**may be re-evaluated with one of the aqueous calibra tion standards to assure**  **complete separation of all target analytes.**

**NOTE : Traces of water in the GC/FT-IR interface are acc**  **eptable. However, the repeated injection of 1.0-μL aqueous samples may e**  **ventually destroy the**

**KBr window used for FT-IR detection. Care should b e taken in deciding the**  **valve switching time so that the KBr window is expo sed to only trace**  **amounts of water and target analytes that elute wit h retention times just** 

**after water are not missed.**

**11.4.2.3 If the TCD is proven to have adequate s ensitivity for a** 

**particular analysis, it may be used as the prime de tector once the target analytes**  **are identified using the FT-IR detector. When the TCD is used as the prime** **SW-846 Update V 8430 - 9 Revision 1 July 2014**  **detector, the switching valve should remain in the position which diverts the sample**  **away from the KBr window.**

**11.4.3 Sample analysis – Analyze the samples, bla nks, spiked blanks, and**  **spiked matrix samples by injecting 1-μL aliquots in to the GC and switching to the FT-IR**  **spectrometer at the previously determined time. Di lution of the sample may be necessary**  **to adjust the analyte concentration to within the w orking range of the calibration curve. If**  **dilution is necessary, note which samples were dilu ted in the final report and make the**  **appropriate calculation adjustments.**

**11.4.4 GC/FT-IR identification – Visually compare the analyte IR spectrum**  **versus the search library spectrum of the most prom ising on-line library search hits.**  **Report, as identified, those analytes with IR frequ encies for the five (maximum number)**  **most intense IR bands (S/N ≥ 5) which are within ±5 .0 cm**  **-1 of the corresponding bands in**  **the library spectrum. Choose IR bands which are sh arp and well resolved. The software**  **used to locate spectral peaks should employ the pea k "center of gravity" technique. In**  **addition, the IR frequencies of the analyte and lib rary spectra should be determined with**  **the same computer software.**

**12.0 DATA ANALYSIS AND CALCULATIONS**

**12.1 Calculations**

**12.1.1 Calculate the CF for each calibration stan dard and determine the percent**  **relative standard deviation (%RSD) using the extern al standard calibration procedure in** 

**Sec. 11 of Method 8000.**

**12.1.2 Calculation of the concentration of analyt es using the external standard**  **calibration procedure is provided in Sec. 11 of Met hod 8000.** 

**12.1.3 Results should be reported in units commen surate with their intended use** 

**and all dilutions should be taken into account when computing final results.** 

**13.0 METHOD PERFORMANCE**

**13.1 No LLOQ data are available.**

**13.2 Minimum Identifiable Quantities**

**13.2.1 The MIQ is defined as the minimum quantity that must be injected to**  **result in a spectral match that has the correct com pound identification in the top 5 spectral**  **matches. The MIQ will vary depending on instrument sensitivity and sample matrix** 

**effects.**

**13.2.2 The MIQ range for CE, BCEE, EG, 2CEE, and DEG in organic-free**  **reagent water by direct aqueous injection goes from a low of 46 ng for BCEE to a high of**  **120 ng for EG. SW-846 Update V 8430 - 10 Revision 1**  **July 2014 14.0 POLLUTION PREVENTION** 

**14.1 Pollution prevention encompasses any technique that reduces or eliminates the**  **quantity and/or toxicity of waste at the point of g eneration. Numerous opportunities for pollution**  **prevention exist in laboratory operation. The Envi ronmental Protection Agency (EPA or the**  **Agency) has established a preferred hierarchy of en vironmental management techniques that**  **places pollution prevention as the management optio n of first choice. Whenever feasible,**  **laboratory personnel should use pollution preventio n techniques to address their waste**  **generation. When wastes cannot be feasibly reduced at the source, the EPA recommends**  **recycling as the next best option.**

**14.2 For information about pollution prevention th at may be applicable to laboratories** 

**and research institutions consult** Less is Better: Laboratory Chemical Management for Waste

Reduction **, a free publication available from the ACS, Commit tee on Chemical Safety,**  **http://portal.acs.org/portal/fileFetch/C/WPCP_01229 0/pdf/WPCP_012290.pdf** 

**.**

**15.0 WASTE MANAGEMENT**

**The EPA requires that laboratory waste management p ractices be conducted consistent**  **with all applicable rules and regulations. Laborat ories are urged to protect air, water, and land**  **by minimizing and controlling all releases from hoo ds and bench operations, complying with the**  **letter and spirit of any sewer discharge permits an d regulations and complying with all solid and**  **hazardous waste regulations, particularly the hazar dous waste identification rules and land**  **disposal restrictions. For further information on waste management, consult**  The Waste Management Manual for Laboratory Personnel **available from the ACS at the web address listed**

**in Sec. 14.2 above.**

**16.0 REFERENCES**

**1. Payne, W.D. and Collette, T.W., "Identification of Bis(2-chloroethyl)ether Hydrolysis**  **Products by Direct Aqueous Injection GC/FT-IR,"** J. of High Res. Chrom. **, 12, 693-696,**

**1989.**

**17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION D ATA** 

**The following pages contain the tables referenced b y this method.** **SW-846 Update V 8430 - 11 Revision 1 July 2014**  **METHOD 8430**

**ANALYSIS OF BIS(2-CHLOROETHYL)ETHER AND HYDROLYSIS PRODUCTS** 

**BY DIRECT AQUEOUS INJECTION SW-846 Update V 8430 - 12 Revision 1**  **July 2014 TABLE 1** 

**QC of FT-IR Spectrometer**

**T.1 Equipment Adjustments and Maintenance**

**T.1.1 Mirror alignment – Adjust the interferometer mirrors to attain the most intense**  **signal. Data collection should not be initiated un til the interferogram is stable. If necessary,**  **align the mirrors prior to each GC/FT-IR run.**

**T.1.2 Interferometer – If the interferometer is ai r-driven, adjust the interferometer drive air**  **pressure to manufacturer's specifications.**

**T.1.3 Lightpipe – The lightpipe and lightpipe wind ows should be protected from moisture** 

**and other corrosive substances at all times. For t his purpose, maintain the lightpipe**  **temperature above the maximum GC program temperatur e but below its thermal degradation**  **limit. When not in use, maintain the lightpipe tem perature slightly above ambient. At all times**  **maintain a flow of dry, inert, carrier gas through the lightpipe.** 

**T.1.4 Beamsplitter – If the spectrometer is thermo stated, maintain the beamsplitter at a**  **temperature slightly above ambient at all times. I f the spectrometer is not thermostated,**  **minimize exposure of the beamsplitter to atmospheri c water vapor.** 

**T.2 Centerburst intensity and mercury/cadmium/tellu rium (MCT or HgCdTe) detector check** 

**T.2.1 With an oscilloscope, check the MCT detector centerburst intensity versus the**  **manufacturer's specifications. Increase the source voltage, if necessary, to meet these**  **specifications. For reference purposes, laboratori es should prepare a plot of time versus**  **detector voltage over at least a five-day period.**

**T.2.2 If the centerburst intensity is 75 percent o r less of the mean intensity of the plot**  **maximum obtained by the procedure, install a new so urce and check the MCT centerburst with**  **an oscilloscope versus the manufacturer's specifica tions (if available). Allow at least five hours**  **of new source operation before data acquisition.**

**T.2.3 Align test – With the lightpipe and MCT dete ctor at thermal equilibrium, check the**  **intensity of the centerburst versus the signal temp erature calibration curve. Signal intensity**  **deviation from the predicted intensity may mean the rmal equilibrium has not yet been achieved,**  **loss of detector coolant, decrease in source output , or a loss in signal throughput resulting from**  **lightpipe deterioration.**

**T.3 GC/FT-IR sensitivity**

**T.3.1 Capillary column interface sensitivity test – Install a 30 m x 0.32 mm fused silica**  **capillary column coated with 1.0 μm of DB-5 (or equ ivalent). Set the lightpipe and transfer lines**  **at 280 °C, the injector at 225 °C and the GC detect or at 280 °C (if used). Under splitless Grob**  **type or on-column injection conditions, inject 25 n g of nitrobenzene and dissolve in 1 μL of**  **methylene chloride. The nitrobenzene should be ide ntified by the on-line library software search**  **within the first five hits (nitrobenzene should be contained within the search library).** 

**T.3.2 One hundred percent line test – Set the GC/F T-IR operating conditions to those**  **employed for the sensitivity test (see Sec. T.3.1). Collect 16 scans over the entire detector**  **spectral range. Plot the test and measure the peak -to-peak noise between 1800 and 2000 cm**  **-1**

**. This noise should be less than or equal to 0.15 per**  **cent. Store this plot for future reference. SW-846 Update V 8430 - 13 Revision 1**  **July 2014 T.3.3 If the GC/FT-IR was purchased before 1985, t**  **here may be a temperature effect at the interface. To account for this, prepare a plot**  **of lightpipe temperature versus MCT centerburst intensity (in volts or other vertical h**  **eight units). This plot should span the temperature range between ambient and the lightpipe**  **thermal limit in increments of about 20 °C. Use this plot for daily QA/QC (see Sec. T.2.3)**  **. Note that modern GC/FT-IR interfaces (1985 and later) may have eliminated most of this t**  **emperature effect.**

**T.4 Frequency calibration – At the present time, no consensus exists within the spectroscopic**  **community on a suitable frequency reference standar d for vapor-phase FT-IR. One reviewer**  **has suggested the use of indene as an on-the-fly st andard.** 

**T.5 Single beam test – With the GC/FT-IR at analysi s conditions, collect 16 scans in the single**  **beam mode. Plot the co-added file and compare with a subsequent file acquired in the same**  **fashion several minutes later. Note if the spectro meter is at purge equilibrium. Also check the**  **plot for signs of deterioration of the lightpipe po tassium bromide windows. Store this plot for** 

**future reference. SW-846 Update V 8430 - 14 Revision 1**  **July 2014 Appendix A** 

**Changes in this version from the December 1996, Rev ision 0.** 

**1. Improved overall method formatting for consisten cy with new SW-846 methods style**  **guidance. The format was updated to Microsoft Word .docx. This includes the additions**  **of all sections required by the new format.**

**2. Many minor editorial and technical revisions wer e made throughout to improve method**  **clarity.**

**3. The revision number was changed to one and the d ate published was changed to July** 

**2014.**

**4. This appendix was added showing changes from the previous revision.** 

**5. The "Quality Control of FT-IR Spectrometer" sect ion previously referred to as Appendix**  **A was renamed to TABLE 1 to keep consistency in for mat with other methods in Update** 

**V.**

**6. The flowchart on page 11 was updated to reflect the current section numbers.**