Trace Metal Considerations when Phosphorus Removal ... WWOA...Trace Metal Considerations when...

Trace Metal Considerations when Phosphorus Removal Chemicals

are Used

Rick Mealy, Program Chemist (DNR Certification Services)

1

What’s the hub, bub?

Water weighs 8 lbs/gallon!

2/43

3/43

Does it work? (Watertown data)

Did not get down to 0.1 in limited trial, but… … up to 75% reduction in effluent Total P … up to 85% reduction in effluent PO4

4/43

Solution: A whole other talk

Theory: Communities of Watertown’s size could get below 0.1 as long as they don’t have a problem with Soluble non- reactive phosphorus (SNRP)

0.657

0.061

SNRP 0.596 mg/L

5/43

So…if it works…what’s the issue?

6/43

http://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwj85NydxaXWAhWq7YMKHRwlDUQQjRwIBw&url=http://fundraisingcoach.com/2016/06/23/telling-stories-move-donors-give/&psig=AFQjCNHd9WOLeimJAqOBfUP7Az2lsMkNkg&ust=1505507988025272

Kewaskum’s experience… • About 2 years ago we learned that products were

available that contained over 30% Cerium (Ce).

• Note: EPA ICP method 200.7 warns of Ce interference. (but SW-846 6010 does not!)

• In late summer 2016, Kewaskum had trouble landspreading its biosolids; it was failing for Arsenic

• 3 different labs used; all said it exceeded arsenic (As) standards or that results were funky.

• Kewaskum never had As in biosolids before. • But they were taking in a source using SorbX-100.

• Checked with labs. No correction for Ce on As. • Once correction applied, As “disappeared”.

7/43

Kewaskum's Arsenic Results (mg/kg dry weight) Received Lab Result Tech. Line 07/21/16 …4950 155 ICP 08/10/16 …4950 161 ICP 08/18/16 …6460 < 24 ICP Noted Ce @36,000 mg/kg

08/18/16 …4950 < 3.0 ICP/MS 09/09/16 …2750 192 ICP/MS 210 ICP/MS 09/12/16 …6460 < 24 ICP 193.7 nm

Noted Ce at 145 mg/L, potential low bias due to over correction …6460 87.9 ICP 189 nm …6460 87.13 ICP 189 nm …6460 91.33 ICP 189 nm 09/14/16 …3790 84.9 ICP Outfall 002-1G

…3790 90.2 ICP Outfall 002-2G

…3790 88.9 ICP Outfall 002-3G

NR 204 limit 75 mg/kg

???

???

???

???

???

??? 8

• Digested & analyzed using normal solids method.

• Upon learning about the Ce levels in the samples,

• developed new solids method; added two As λs (188.979 & 193.696) and a Ce λ.

• Ce level in the samples was ~45,000 ppm.

• Corrected for this interference on both As λ s.

• 193.696 λ needed a huge correction

• 188.979 did not need much of a correction.

• Since, results from the two λs didn’t agree… suspect an interference causing high As bias at 188.979 λ.

• Analyzed by ICP-MS to better assess the interference. 9

9/43

10

10/43

❶ ➋ ➌ ❹ ❺

11

https://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwiYzujejrHWAhUp0YMKHYevApgQjRwIBw&url=https://www.ptable.com/&psig=AFQjCNFCU23OZlYpQRKk9NdVosNQy_goZw&ust=1505905871598742



http://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwi14ueuzrPWAhWI64MKHW4qB88QjRwIBw&url=http://www.heavymetalmagazinefanpage.com/&psig=AFQjCNFUlMdZlccpCAgJOlG6-HuABaU0hA&ust=1505991597109245

How to determine what’s in it

• High resolution ICP/MS is a powerful tool to identify and quantify with certainty any elements present.

• Unfortunately, few labs have this capability. The State Lab of Hygiene, however, has the instrument and a talented staff to run it.

• We used this as a first step to absolutely determine what elements are present in the Neo product as well as concentration levels

12/43

Rare Earths (RE) in RE300/100

Comparison of Rare Earth Elements in RE-300 and RE-100

µg/L REE

1e-1 1e+0 1e+1 1e+2 1e+3 1e+4 1e+5 1e+6 1e+7 1e+8 1e+9

Ce

Gd

Tb

Pr

La

Yb

Nd

Lu

Eu

Sm

Tm

Dy

Er

Ho

RE-300RE-100

(ranked by RE-300 levels)


µg/L REE

1e-1 1e+0 1e+1 1e+2 1e+3 1e+4 1e+5 1e+6 1e+7 1e+8 1e+9

Ce

Gd

Tb

Pr

La

Yb

Nd

Lu

Eu

Sm

Tm

Dy

Er

Ho

RE-300RE-100



µg/L REE

1e-1 1e+0 1e+1 1e+2 1e+3 1e+4 1e+5 1e+6 1e+7 1e+8 1e+9

Ce

Gd

Tb

Pr

La

Yb

Nd

Lu

Eu

Sm

Tm

Dy

Er

Ho

RE-300RE-100



µg/L REE

1e-1 1e+0 1e+1 1e+2 1e+3 1e+4 1e+5 1e+6 1e+7 1e+8 1e+9

Ce

Gd

Tb

Pr

La

Yb

Nd

Lu

Eu

Sm

Tm

Dy

Er

Ho

RE-300RE-100

(ranked by RE-300 levels) 0.001 0.01 0.1 1 10 100 1,000 1% 10% Ppm/% Rare Earth Metals

WI State Lab of Hygiene data

14 Rare Earth Elements identified!

13/43

Other Elements in RE300/100

Elem

en

t C

on

cen

tratio

ns in

R

E-300

(n

on

-R

EE

)

Na

SC

aP

KM

gS

iA

lL

iB

aF

eS

eZ

nP

bS

rB

Cr

NiH

gC

uT

iM

nB

eW

VS

bP

tR

bM

oH

fS

nU

YC

sC

oC

dA

gR

uP

dS

cT

lT

aT

hR

hN

b

µg/L

1e-2

1e-1

1e+

0

1e+

1

1e+

2

1e+

3

1e+

4

1e+

5

ug/L 0.01 0.1 1 10 100 1,000 1% 10% | | | | | | | |

Na -

S -

Ca -

P -

K -

Mg -

Si -

Al -

Li

Y -

Y (Yttrium) 5-10 ppb in RE 300 300-500 ppb in RE 100

14/43

Metals testing 101

Now we need a low tech summary of metals

testing and ICP Optical Emission Spectrometry

15/43

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Metals instrumentation

FLAA 1,700-2,400 C

GFAA 2,000-2,500 C

ICP ~8,000 C

16/43

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http://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwj1r5T8zOvVAhWIyoMKHSJHAq0QjRwIBw&url=http://www.viridiangold.com/jewelry-size-comparison.html&psig=AFQjCNGq3QT-H__B7w04GoCJDKHOcDJBEg&ust=1503517390820049

+

Torch

Sample, containing infinite numbers of molecules, is aspirated into the ICP torch

Inside the plasma, the sample is initially vaporized. At this point all molecules are atomized.

Then, atoms collide with electrons and Argon ions causing the atoms to become excited

The atoms naturally drop back to ground state, releasing energy in the form of light

The wavelength generated is characteristic of the particular element

Basic theory

17

Relative hotness

Molten lava : 900-1200 C F-35 full afterburner 1900 C

Welders torch 3,500 C

Sun’s surface 10,000 C

Lightning 20,000 to 30,000 C

Earths core 6,000 C

8,000 C

18/43

OK…so ICP is hot…

Why do we care about how hot something is?

• The ICP torch is really plasma energy.

• EVERYTHING is atomized.

• Background matrix interferences are essentially non-existent (what could survive 8,000 C?).

• The only interferences we need to worry about are spectral interferences.

• Spectral interference occurs when an emission line from one element “bleeds” into another element’s emission.

19/43

Spectral interference 101

V

292.416 292.385 292.369 292.401

292.448 292.432 292.463

V

Oh sure…looks nice and simple when all you analyze is a standard…

20/43

Spectral interference 101

Oh sure…looks nice and simple when all you analyze is a standard…

V

V

Fe Cr

Mo

292.416 292.385

292.369 292.401 292.448

292.432 292.463

…but when you have a sample …with real elements …having varied concentrations…

21/43

Spectral overlap

Spectral overlap is simply when another element has an emission line very close to another target element, and as concentration increases, it “bleeds” into the other element’s window.

Adamantium X

250 ppm X

Adamantium X

100 ppm X

Adamantium X

50 ppm X

Adamantium X

500 ppm X

At 50 ppm, element X has no impact on Adamantium

But at 500 ppm, X’s emission bleeds into and is counted as Adamantium

22/43

Background correction issues Improper background correction can also occur. If a background correction point is placed where an interferent emits, it can cause peak reduction.

-------------

------

Scenario A Nothing present, background correction point becomes peak integration baseline.

Scenario B 1 background point. If an interferent exists, the baseline is re-set, creating negative peaks.

Scenario C 2 background points. If interferents affect both sides of the target peak, the peak can be shaved off and a new baseline created.

A B C

23/43

Correcting for interferences

• Analyze a bunch of individual pure element standards.

• Determine what elements should be absent—but aren’t

Inter-element

Correction

(IEC) Factors!

24/43

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Flashback to Kewaskum data

λ As 188.979

λ As 193.696

ICP (2 labs)

ICP/MS (1 lab) As m/z 75

Nd++ m/z 150

Sm ++ m/z 150

λ La 188.922

λ Ce 193.721

150Nd 149.920

150Sm 149.917

75As 74.921

150Nd 74.960

150Sm 74.959

25/43

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https://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwiCvLLmwLvWAhXH5YMKHQJnA4wQjRwIBw&url=https://buffy2ville.deviantart.com/art/Arrow-Season-4-Logo-Png-577532464&psig=AFQjCNET9iJFwHb2_-ZHjZrOSqqYiDSKdw&ust=1506262901806523

Lanthanum (La) Direct overlap

Problems with Arsenic Detection: https://www.aiha.org/aihce06/handouts/po122gunderson.pdf

WI State Lab of Hygiene data

Cerium (Ce) Background correction issue

188.979 line

Arsenic 2 ppm

193.696 nm Cerium 400 ppm

193.696 line

26/43

Direct overlaps are VERY difficult… what if BOTH are present?

Arsenic 188.979 line

Ce 400 ppm

La 100 ppm

La 50 ppm

As 2 ppm

La 20ppm

Fe 300 ppm

2 background correction points Direct overlaps are

VERY difficult to correct

for

27/43

Arsenic 193.696 line (1 pt)


1 background correction point

Ce 400 ppm

As 2 ppm

28/43

Arsenic 193.696 line (2 pts)

Ce 400 ppm

As 2 ppm

Fe 300 ppm 2 background correction points


La 100 ppm La 50 Pr 10 La 20 S100

29/43

Putting what we learned to work • We wanted to analyze biosolids data of facilities

using RE100/300 and look at data with and without proper correction.

• We also wanted to look at effluent trace metals data to see if any of the REEs appear in the effluent (and thus may need correction) or potentially lead to permit issues.

30/43

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Effluents: Good News!

EHD-Metals ICP-OES Data of WWTP Effluents (ug/L

these are interference corrected


Element

T own of

Norway

Village of

Sussex Wate rtown Juneau

Al 396.153 R 26.81 10.41 29.18 71.95

Sb 217.582 ND ND ND ND

As 188.979 ND ND ND ND


Ba 233.527 44.92 54.54 64.71 13.57

Be 313.107 ND ND ND ND

B 249.677 171.18 126.33 465.23 100.90

Cd 226.502 ND ND ND ND

Ca 317.933 R 92,861.39 88,295.96 86,059.95 50,078.76

Cr 205.560 ND ND 1.63 ND

Co 228.616 ND ND ND ND

Cu 324.752 7.86 13.13 15.79 10.55

Fe 238.204 R ND ND 150.00 ND

Pb 220.353 ND ND ND ND

Mg 279.077 R 52,316.17 39,551.09 47,796.95 34,634.26

Mn 257.610 21.21 5.12 32.99 ND

Mo 202.031 3.78 ND ND ND

Ni 231.604 2.62 2.09 7.91 2.72

P 213.617 346.09 463.40 321.00 875.94

K 766.490 R 7.84 7.94 33.94 49.72

Se 196.026 ND ND ND ND

Ag 328.068 ND ND ND ND

Na 589.592 R 302,984.69 219,168.01 272,587.82 269,568.59

Sr 407.771 R 539.65 7,632.94 339.82 1,524.00

S 181.975 7,513.99 5,275.65 8,637.19 10,244.24

Tl 190.801 ND ND ND ND

Sn 189.927 ND ND ND ND

Ti 336.121 ND ND ND ND

V 292.402 ND ND 1.47 1.11

Zn 206.200 20.83 17.60 30.18 14.91

Ce 413.764 R ND 11.53 1640.25 ND

S 181.975 R 17,778.75 18,553.69 57,080.14 33,126.28

Gd 342.247 R ND ND ND ND

La 408.672 R ND ND ND ND

Nd 406.109 R ND ND ND ND

Pr 390.844 R ND ND ND ND

Sm 359.260 R ND ND ND ND

Ho 345.600 R ND ND ND ND

EHD-Metals ICP-OES Data of WWTP Effluents (ug/L)


Element

T own of

Norway

Village of


Al 396.153 R 26.81 10.41 29.18 71.95




Ba 233.527 44.92 54.54 64.71 13.57


B 249.677 171.18 126.33 465.23 100.90


Ca 317.933 R 92,861.39 88,295.96 86,059.95 50,078.76

Cr 205.560 ND ND 1.63 ND


Cu 324.752 7.86 13.13 15.79 10.55

Fe 238.204 R ND ND 150.00 ND


Mg 279.077 R 52,316.17 39,551.09 47,796.95 34,634.26

Mn 257.610 21.21 5.12 32.99 ND

Mo 202.031 3.78 ND ND ND

Ni 231.604 2.62 2.09 7.91 2.72

P 213.617 346.09 463.40 321.00 875.94

K 766.490 R 7.84 7.94 33.94 49.72



Na 589.592 R 302,984.69 219,168.01 272,587.82 269,568.59

Sr 407.771 R 539.65 7,632.94 339.82 1,524.00

S 181.975 7,513.99 5,275.65 8,637.19 10,244.24




V 292.402 ND ND 1.47 1.11

Zn 206.200 20.83 17.60 30.18 14.91

Ce 413.764 R ND 11.53 1640.25 ND

S 181.975 R 17,778.75 18,553.69 57,080.14 33,126.28









Element

T own of

Norway

Village of


Al 396.153 R 26.81 10.41 29.18 71.95




Ba 233.527 44.92 54.54 64.71 13.57


B 249.677 171.18 126.33 465.23 100.90


Ca 317.933 R 92,861.39 88,295.96 86,059.95 50,078.76

Cr 205.560 ND ND 1.63 ND


Cu 324.752 7.86 13.13 15.79 10.55

Fe 238.204 R ND ND 150.00 ND


Mg 279.077 R 52,316.17 39,551.09 47,796.95 34,634.26

Mn 257.610 21.21 5.12 32.99 ND

Mo 202.031 3.78 ND ND ND

Ni 231.604 2.62 2.09 7.91 2.72

P 213.617 346.09 463.40 321.00 875.94

K 766.490 R 7.84 7.94 33.94 49.72



Na 589.592 R 302,984.69 219,168.01 272,587.82 269,568.59

Sr 407.771 R 539.65 7,632.94 339.82 1,524.00

S 181.975 7,513.99 5,275.65 8,637.19 10,244.24




V 292.402 ND ND 1.47 1.11

Zn 206.200 20.83 17.60 30.18 14.91

Ce 413.764 R ND 11.53 1640.25 ND

S 181.975 R 17,778.75 18,553.69 57,080.14 33,126.28








Minerals

RE Elements

31

31/43

Effluent levels (ppb)

7,840 7,940 33,940 49,720

32

32/43

Semi-final data Biosolids (mg/kg)

• xxxx

33

33/43

Semi-final data Biosolids (mg/kg)

• Arsenic: Significant changes when IECs (inter-element correction factors) are applied.

• Still disagreement between the 2 lines. • Suspect background correction issues.

61.0

34

34/43

FINAL data Biosolids (mg/kg)

Single background correction point for both wavelengths. 193 is preferred wavelength due to interference from La Unique IEC table developed for each sample based on the concentrations of elements found in that sample

Table 1 Ceiling Concentrations Pollutant Ceiling concentrations (milligrams per kilogram—ppm) (dry weight) Arsenic 75 Cadmium 85 Copper 4300 Lead 840 Mercury 57 Molybdenum 75 Nickel 420 Selenium 100 Zinc 7500

35

35/43

Uncorrected After correction Outfall 002-1G 84.9 9.58 Outfall 002-2G 90.2 8.77 Outfall 002-3G 88.9 9.99 Average 88 9.11

Initial results

Follow-up results (line 193.696)

NR 204 limit 75 mg/kg

193

36

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How SLH addressed the problems Calibration: added 15 REEs/25 wavelengths (based on HR ICP/MS). Biosolids issues- Ce 500 ppm, P 700 ppm Fe 750 ppm IEC changes required for 10 elements High levels of Y in RE100 (less so in RE300) Y used as internal standards (IS) to adjust element data. Bias in IS will result in biased results. 500 ppm Ce required huge IECs for Nd and Pr “Synergistic” interferences: Compound 1 affects Arsenic, but Compound 2 interferes (high bias) w/ compound 1 (e.g. Pr)

37/43

Communicate! 38/43

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https://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwiV2saLkNfVAhVq2IMKHX4hBjAQjRwIBw&url=https://holykaw.alltop.com/how-to-effectively-communicate-with-your-remote-employees&psig=AFQjCNGhFF4Eq8IYPswmBvfR53QWfa6nlw&ust=1502813760358696

https://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwiPipmGrrvWAhUl2oMKHRGEDCcQjRwIBw&url=https://www.slideshare.net/CSSCenter/the-leads-are-coming-innow-what-do-we-do&psig=AFQjCNG5tC9FuJqZ7MG2uteL8bsUcq8y7Q&ust=1506257829983899

Communication - WWTP role When you send biosolids samples to a contract

lab, you need to:

• TELL the lab if you use(d) RE100 or RE300

• ASK if they plan to use ICP (or GFAA or ICP/MS)

• Verify that they understand and correct for interferences due to REE

• If results for Arsenic appear to be biased high, verify that the lab applied corrections for REEs.

• The lab should understand. If they do not, you may want to consider using a different lab.

39/43

Communication – Lab role

When you receive biosolids samples: • ASK if any phosphorus-complexing chemicals were used

(and which)…or if the facility received flow/solids from a plant that did.

If RE100 or RE300 were used • Review pre-RE100/300 data (if you have it) • Review historical levels & dosage rate vs. flow • Arsenic: Use the 193.696 nm line vs. 188.979 nm • Use only a single background correction point • Ensure proper corrections are in place • Create a special ICS to assess effectiveness of IECs

40/43

Conclusions RE100/RE300 DO effectively remove phosphorus. These products DO pose challenges for ICP & ICP/MS But…. The challenges can be overcome … …as long as you know to address them GFAA= slow (8 elements= 8 runs) ICP =faster/ less matrix interferences than GFAA ICP/MS, while a viable option, is overkill … like hunting squirrels with an elephant gun

41

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http://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwiLpZ2v0rHWAhVo7oMKHRwVBw8QjRwIBw&url=http://www.backyardsquirrels.com/category/feeding-squirrels/&psig=AFQjCNEQlGrzyQbUH2MyRLK6tpniNPfjXw&ust=1505924031552312

It ain’t over ‘till…. • Just last week….

• Facility “X” exceeded the Se standard for its 3rd QTR biosolids: 116 mg/kg

• QTR 1 was 8.1 mg/kg; QTR 2 was 12 mg/kg. Our data collected 2.5 wks earlier also indicated 8.2.

• The only thing that changed in QTR 3 was a pilot test using RE-300. Hmmmm…

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http://www.google.com/url?sa=i&rct=j&q=&esrc=s&source=images&cd=&cad=rja&uact=8&ved=0ahUKEwizr7bJjrfWAhWCyIMKHR36ChgQjRwIBw&url=http://tvtropes.org/pmwiki/pmwiki.php/Main/BlackBox&psig=AFQjCNEGtusVmgEw9eJAYsNOWnun_baJmQ&ust=1506111998485865

State Lab of Hygiene ICP: DeWayne Kennedy-Parker, Kevin Kaufman ICP/MS: Martin Shafer, Pat Gorski, Christa Dahman, Pam Skaar, Joel Overdier

DNR – State Lab Liaison Zana Sijan

Neo Materials Pam Cornish WWTP Facilities PJ Nolan (Norway Sewer Utility #1) Tim Hayden (Juneau WWTP) Kevin Freber (Watertown Water/Wastewater Utilities) Dennis Wolf (Sussex WWTP) Ben Propson (Kewaskum)

This was a team effort!

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