What happens to the Samples after collection?
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1 What happens to the Samples after collection? Just what DOES the lab do with samples after they are collected? Denise L. Seman City of Youngstown Wastewater
2 Explanation of sample types
3 Grab A single, one time grab of sample
4 Grab analysis of ph, temperature, cyanide, total phenols, residual chlorine, oil and grease, fecal coliform (including E. coli), and Enterococci (previously known as fecal streptococcus ), or volatile organics, grab samples must be collected for those pollutants. 40 CFR Part 136
5 Composite a a 24-hour composite sample, using a minimum of four (4) grab samples, must be used unless specified otherwise at 40 CFR Part 136
6 Composite Multiple samples grabbed, then placed together into the same container
7 Youngstown sampler ISCO external ISCO internal
8 Struthers sampler Sigma Sigma controller
9 Carboys
10 Characteristics and sampling frequency are determined by the NPDES permit
11 Common characteristics include: CBOD TSS NH3 Total Phosphorous Temperature ph DO
12 Characteristics we monitor/test for: Temperature, DO, TSS, Oil & Grease Nitrogen- Ammonia, Nitrate-nitrite, TKN Total Phosphorous, Hexavalent Chromium Free Cyanide, Chloroform, CBOD Flow rate, Fecal coliforms, Mercury
13 Characteristics we monitor/test for: Total residual chlorine Metals, total recoverable: Nickel, Silver, Zinc, Cadmium, Lead, Chromium, Copper Bioassay: Acute & Chronic toxicity both fat-head minnows and water fleas
14 Grab Samples
15 Daily ph, temperature and dissolved oxygen (D.O.) check to ensure the automatic system stays in calibration for both the raw and final. Grab samples, analyzed within 15 minutes of collection/ delivery to lab
16 ph and temperature are checked on a Thermo scientific 5 star meter/ probe
17
18 D.O. D.O. is checked on a YSI meter/ probe Also Also commonly used are Thermo-Orion meter/ probe combo
19 Youngstown: YSI system Geneva: Thermo-Orion system
20 Chlorine residual is tested/ monitored 3 times daily during the summer months to report a maximum discharge concentration
21 Chlorine concentration is also checked once daily at the base of the cascade, and again after the contact tanks to ensure adequate chlorine is being applied for disinfection.
22 Chlorine residual is checked by amperometric titration Permit limit is mg/l, ML is mg/l according to the EPA. Violations do not occur until the ML has been exceeded. Grab samples, analyzed within 15 minutes of collection/ delivery to lab
23
24 Fecal coliforms, total coliforms and E. coli are daily tests during the summer months Samples must be analyzed within 6 hours of collection. Samples are incubated for 24 hours before reading.
25
26 Filtering set Magnetic funnel Glass funnel
27 Oil & Grease samples are grab samples, but can be preserved with acid to a ph <2 and stored for up to 28 days. We do Oil & grease by EPA method 1664A, automated solid phase extraction with n-hexanen Can also be done by liquid to liquid extraction
28
29
30
31 Composite
32 Composite samples are brought into the lab, where they are split out according to the requirements for the day s s analysis.
33
34
35
36 Total suspended solids analysis are performed daily Samples can be held, unpreserved, for up to 28 days at </= 6 o C Samples are analyzed in accordance with SM 2540-D.
37
38 CBOD s s are collected daily. Samples can be held, unpreserved, for up to 48 hours after collection at </= 6 o C Sample sets are put on for analysis on Monday, Wednesday and Friday. There is a 5 day incubation period
39 BOD incubators
40 Metals samples: Cd, Cr, Cu, Pb, Ni, Zn, Ag for raw and final are collected once every 2 weeks. Samples are preserved with acid to a ph <2 and can be held for up to 6 months. Samples are digested for total recoverable metals in a programmable hot block, in accordance with EPA method 200.7
41 Hot block digesters Youngstown Geneva
42 Sludge metals, composited, are prepped in the hot block, but the digestion step includes heating with a 30% hydrogen peroxide solution to break any organic bonds Sludge metals are collected once a month, by compositing over an 8 to 16 hour period Sludge is analyzed for As, Be, Cd, Cr, Cu, Pb, Ni, Mo, Se, Zn
43 Prepped, digested metals samples are analyzed by ICP, in accordance with EPA method Metals can also be analyzed by AA
44 ICP
45 AA Struthers Flame AA Struthers Furnace AA
46 Phenols (industrial and background samples only) Batch analysis, including a digested blank, standard, duplicate and spike Analyzed on the Westco Smartchem
47
48 Smartchem Spec
49 Specs Struthers Geneva
50 Also analyzed on the Westco Smartchem: Hexavalent Chromium Nitrate-nitrite TKN Total Phosphorous
51 TKN and total phosphorous digested on Westco Smartdigest (in Youngstown) Other digestion apparatus for TKN are hot block system
52 TKN digestion Smart block Hot block
53 Mercury samples (industries, background, and sludge) are prepped automatically in the Environmental Express Autoblock II Analyzed by cold vapor analysis on a Leeman Labs Analyzer
54
55
56 Glassware for mercury, total metals and total phosphorous acid cleaned in the Milestone Traceclean
57
58 After all analysis is complete, samples are dumped, containers are cleaned and the process begins again.
59 Questions?
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