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pH and ICP Techniques. Clemson. Scoop 2 checks One blank Double scoop 6 samples Tag set with lab number, check, and blank positions. pH quality control checks. Two QC check samples Two samples at beginning, middle, and end of set Cross Check electrodes #1 and #2 . 1. 2. 3.

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pH and ICP Techniques

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Ph and icp techniques l.jpg

pH and ICP Techniques

Clemson


Ph quality control checks l.jpg

  • Scoop 2 checks

  • One blank

  • Double scoop 6 samples

  • Tag set with lab number, check, and blank positions

pH quality control checks


Quality control row l.jpg

  • Two QC check samples

  • Two samples at beginning, middle, and end of set

  • Cross Check electrodes #1 and #2

1

2

3

Quality control row


End of run verification l.jpg

ck

  • Check both QC check values at beginning and within set

  • Check all double scooped samples at beginning, middle, and end of set

  • Buffer run - checks

  • Buffer run - blank (1:1, water:buffer)

End of run verification


Maintenance l.jpg

  • Friday

    • clean out electrode filling solution

    • fill with water

  • Ultrasonic cleaner

  • Store in buffer pH 7 for the weekend

Maintenance


Maintenance cont l.jpg

  • Monday

    • Take water out of electrode

    • Refill with KCl filling solution

  • Verify flow of KCl through filter

  • Refresh buffer solutions

  • Electrode (from Fisher)

    • Accumet rugged bulb pH combination electrode

    • 13-620-183A

Maintenance – cont.


Ph check values l.jpg

  • Check B data since April 1, 2010

  • 115 continuous reads over a 2.5 month period

  • Rinse pH < 4.5 and > 7.0

  • NAPT value 5.15

  • Lab average 5.15

  • stdev 0.036

pH Check values


Icp quality control checks l.jpg

  • Two checks within the set

  • One blank

ICP quality control checks


Sample entry l.jpg

  • Probe – Leeman Labs

    • Phone: 603-886-8400

    • Part number 902-00017

  • Check all tubing for cleanliness and kinks

  • Change pump winding tube when needed

  • Adjust pump winding clamp - look for smooth flow as sample travels though tube

Sample entry


Nebulizer gas flow l.jpg

  • Aspirate yttrium stock solution

  • Look for the tip of the red bullet

  • Adjust nebulizer gas flow rate

ARCOS

TJA

Nebulizer gas flow


Nebulizer and spray chamber l.jpg

  • Keep clean

    • Take apart to rinse out nebulizer and spray chamber parts

  • TJA – use cleaning wire

  • ARCOS

    • SeaSpray Nebulizer

    • Twister Spray Chamber

    • Cross Flow

ARCOS

ARCOS

TJA

Nebulizer and spray chamber


Torch l.jpg

  • ARCOS – clean as needed – salt buildup

  • TJA – clean ~once a year

TJA

ARCOS

Torch


Setting the flush time arcos crossflow l.jpg

  • Transient scan – run standard

  • Check to see when the peak intensities stabilize

  • Clemson – 35 second total flush

    • 25 seconds at 60 rpm

    • 10 seconds at 30 rpm

25 seconds

P

K

Time (seconds) using pump speed of 60 rpm

Setting the flush timeARCOS - Crossflow


Transient scan on arcos l.jpg

18 seconds

25 seconds

Crossflow spray chamber

Twister spray chamber

Transient scan on ARCOS


Transient scan going to rinse arcos crossflow l.jpg

Options for changing flush time

  • Spray chamber

  • Tubing length

  • Pump speed

  • Sample loop

P – 100 ppm

Ca – 100 ppm

K – 100 ppm

Na – 50 ppm

45 seconds

25 seconds

Time in seconds using pump speed of 60 rpm

Transient scan going to rinseARCOS - Crossflow


Setting the flush time tja l.jpg

  • Run time scan

  • Check time for stability

  • Clemson soil method

    • pump speed 200 rpm

    • flush time 30 seconds

Ca - 40 seconds

Pump speed 175 rpm

Setting the flush time - TJA


Line selection arcos l.jpg

  • Look at several recommended lines

  • Clemson - Ca line – 317.933 for soil

Ca – 396.847Saturated signal

Ca – 315.887

Line selection – ARCOS


Method development arcos l.jpg

  • Set peak position

  • Select clean area for background subtraction

  • Look for uncontaminated blank

Peak position

Cu – 324.754

Blank correction

blank

Method development - ARCOS


Instrument profile and data verification l.jpg

  • Run profile when needed

  • On the AROCS - check intensity of P158.599 line

  • If significant UV intensity drop – clean window and/or lens to optics

  • Check new standard against old

  • Read reference sample at start, mid point, and end of run

  • Verify 2 check samples and blank within set

Instrument profile and data verification


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